水热法制备高百分比α -半水合硫酸钙

L. Fu, W. Xia, Torbjörn Mellgren, M. Moge, H. Engqvist
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引用次数: 10

摘要

α-半水合硫酸钙(α-HH)是一种适合于填充骨空隙的材料。α-HH在医学上的应用,特别是在植入方面,显然需要高百分比的α-HH。以三种不同尺寸和表面形貌的市售二水合硫酸钙(DH、CaSO4·2H2O)为原料,通过水热法合成高倍α-HH。三种DH的中位粒径分别为946.7 μm、162.4 μm和62.4 μm。本文将其命名为DH-L、DH-M和DH-S。合成前对原料的粒度分布、形貌和相组成进行了评价。SEM结果表明,DH-L由不规则大颗粒组成,DH-M和DH-S由片状颗粒组成,其中含有少量小颗粒。在适当的水热合成条件下,DH-L的合成温度为105℃/90 min, HH率可达98.8%;DH-M的合成温度为105℃/30 min, HH率可达96.7%;DH-S的合成温度为100℃/45 min, HH率可达98.4%。合成的HH均为六角形柱状,表明其为α-相HH。起始原料(DH)的粒度和形貌不仅对α-HH的相变速率有显著影响,而且对合成的α-HH的形貌也有显著影响。用合成的α-HH制备了二水硫酸钙胶结剂。二水硫酸钙水泥的最高抗压强度为17.2 MPa。结果表明,水热法制备高纯度α-HH是可行的,该工艺可进一步扩大到工业规模生产。
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Preparation of High Percentage α -Calcium Sulfate Hemihydrate via a Hydrothermal Method
α-calcium sulfate hemihydrate (α-HH) is known to be suitable for application as bone void filler. High percentage of α-HH is obviously needed for medical applications, especially for implantation. Three commercially available calcium sulfate dihydrates (DH, CaSO4·2H2O) with different sizes and surface morphologies were used as starting materials to synthesize high percentage α-HH via a hydrothermal method. The median particle sizes of the three types of DH were 946.7 μm, 162.4 μm and 62.4 μm, respectively. They were named as DH-L, DH-M and DH-S in this paper. The particle size distribution, morphology and phase composition of the raw materials were evaluated before synthesis. SEM results revealed that DH-L consisted of irregular large particles, while DH-M and DH-S were composed of plate-like particles with some small ones. High percentage HH can be obtained with proper synthesis parameters by hydrothermal method, specifically, 105 °C/90 min for DH-L (achieving 98.8% HH), 105°C/30 min for DH-M (achieving 96.7% HH) and 100°C/45 min for DH-S (achieving 98.4% HH). All the synthesized HH were hexagonal columns, demonstrating that they were α-phase HH. The particle size and morphology of starting material (DH) have significant influences on not only the rate of phase transition but also the morphology of the synthesized α-HH. Calcium sulfate dihydrate cements were prepared by the synthesized α-HH. The highest compressive strength of calcium sulfate dihydrate cement was 17.2 MPa. The results show that the preparation of high percentage α-HH is feasible via a hydrothermal method and the process can be further scaled up to industrial scale production.
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