Effect of crystallization heat treatment on the microstructure of niobium-doped fluorapatite glass-ceramics.

Effect of crystallization heat treatment on the microstructure of niobium-doped fluorapatite glass-ceramics.
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DOI:
10.1002/jbm.b.32684
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发表时间:
2012-07
影响因子:
3.4
通讯作者:
Gupta, P. K.
Gupta, P. K.
中科院分区:
工程技术3区
文献类型:
--
作者:
Denry, I.;Holloway, J. A.;Gupta, P. K.

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我们的目标是研究热处理温度和加热速率对显微结构和晶相的影响,并评估用于生物医学应用的铌掺杂氟磷灰石玻璃陶瓷中亚微米氟磷灰石晶体的存在范围。玻璃陶瓷样品通过铸造和在700和1200°C之间使用快速或慢速加热速率进行热处理来制备。用原子力显微镜和扫描电子显微镜对材料的微观结构进行了表征。通过X射线衍射分析晶相。原子力显微镜的铸态玻璃显示,在这个系统中发生非晶相分离。XRD证实了氟磷灰石的存在下,在所有的标本,连同镁橄榄石和顽火辉石在较高的温度。升温速率和热处理温度均强烈影响微观结构和结晶度。当使用缓慢的加热速率和在950和1100°C之间的结晶温度时,获得亚微米氟磷灰石晶体和多边形镁橄榄石晶体的双重显微结构。在1100 ℃以上热处理后,出现针状氟磷灰石晶体。快速的加热速率导致晶体尺寸的增加。热处理温度应保持在1100°C以下,同时缓慢加热,以防止晶体溶解,并保持精细分散的亚微米晶体的双重微结构,而不生长针状晶体。
Our goal was to study the effect of heat treatment temperature and heating rate on the microstructure and crystalline phases and assess the domain of existence of sub-micrometer fluorapatite crystals in niobium-doped fluorapatite glass-ceramics for biomedical applications. Glass-ceramic specimens were prepared by casting and heat treatment between 700 and 1200°C using a fast or a slow heating rate. The microstructure was characterized by atomic force microscopy and scanning electron microscopy. Crystalline phases were analyzed by x-ray diffraction. AFM of the as-cast glass revealed that amorphous phase separation occurred in this system. XRD confirmed the presence of fluorapatite in all specimens, together with forsterite and enstatite at higher temperatures. Both heating rate and heat treatment temperature strongly influenced microstructure and crystallinity. A dual microstructure with sub-micrometer fluorapatite crystals and polygonal forsterite crystals was obtained when slow heating rates and crystallization temperatures between 950 and 1100°C were used. Needle-shaped fluorapatite crystals appeared after heat treatment above 1100°C. Fast heating rates led to an increase in crystal size. Heat treatment temperatures should remain below 1100°C, together with slow heating rates, to prevent crystal dissolution, and preserve a dual microstructure of finely dispersed sub-micrometer crystals without growth of needle-shaped crystals.
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