单相氟磷灰石微晶玻璃晶相特征和生物相容性研究
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摘要
采用熔融-淬火-烧结法制备氟磷灰石微晶玻璃,研究其析晶机制和体外生物相容性。采用X射线衍射(XRD)和场发射扫描电镜(FE-SEM)分析了不同烧结温度下样品的晶相组成和微观结构,利用能量色散X射线光谱仪(EDS)分析了化学成分。结果表明,氟磷灰石是烧结微晶玻璃中的唯一晶相,其晶体可以在较宽的温度范围内析出。显微组织结构致密,显微硬度为644～709 Hv0. 1。氟磷灰石晶体在FE-SEM中有针状和多边形两种形态,多边形是短棒状晶体的横断面。低温下,以固相烧结为主,氟磷灰石析晶以表面析晶为主,晶体生长为针形;高温下玻璃液较多,在保温和冷却凝固过程中析出短棒状晶。在37℃温度下将样品在模拟体液中浸泡14 d,SEM/EDS和FT-IR检测结果表明,样品表面包含磷酸根和羟基的吸收带,形成了羟基磷灰石层,可作为骨或牙齿修复材料。
The crystallization mechanism and in vitro biocompatibility of fluorapatite glass-ceramics prepared by melting-quenching-sintering method were investigated. Phase compositions and the microstructure of the studied samples at different heat treatment temperatures were analyzed by X-ray diffraction( XRD) and field emission-scanning electron microscopy( FE-SEM). Chemical composition was observed and analyzed by energy dispersive X-ray spect-roscopy( EDS). The results show that fluorapatite is the only crystalline phase in the sintered glass-ceramics, and the crystals can be precipitated from the basic glass in relatively wide temperature range. Its microstructure is dense,and Hv0. 1 value is between 644 and 709. The crystal morphology of fluorapatites exhibit two kinds of crystal structure: needle-like and polygonal shapes. The polygon is a cross section of a short columnar crystal.The fluorapatite precipitation follows the surface crystallization mechanism in the solid phase sintering process of low temperature. The columnar fluorapatite precipitate from the liquid phase in the sintering process of holding and cooling. The biocompatibility of crystalline materials was inspected in vitro by immersion in simulated body fluid( SBF) for 14 d at 37 ℃. In vitro bioactivity research indicated the formation of hydroxyapatite layer on the surface of the samples. This was confirmed by SEM,EDS photographs and FT-IR. It is expected to be used as a bone or dental restoration materials.
The crystallization mechanism and in vitro biocompatibility of fluorapatite glass-ceramics prepared by melting-quenching-sintering method were investigated. Phase compositions and the microstructure of the studied samples at different heat treatment temperatures were analyzed by X-ray diffraction( XRD) and field emission-scanning electron microscopy( FE-SEM). Chemical composition was observed and analyzed by energy dispersive X-ray spect-roscopy( EDS). The results show that fluorapatite is the only crystalline phase in the sintered glass-ceramics, and the crystals can be precipitated from the basic glass in relatively wide temperature range. Its microstructure is dense,and Hv0. 1 value is between 644 and 709. The crystal morphology of fluorapatites exhibit two kinds of crystal structure: needle-like and polygonal shapes. The polygon is a cross section of a short columnar crystal.The fluorapatite precipitation follows the surface crystallization mechanism in the solid phase sintering process of low temperature. The columnar fluorapatite precipitate from the liquid phase in the sintering process of holding and cooling. The biocompatibility of crystalline materials was inspected in vitro by immersion in simulated body fluid( SBF) for 14 d at 37 ℃. In vitro bioactivity research indicated the formation of hydroxyapatite layer on the surface of the samples. This was confirmed by SEM,EDS photographs and FT-IR. It is expected to be used as a bone or dental restoration materials.
引文
[1]Suchanek W,Yashima M,Kakihana M,et al.Hydroxyapatite Ceramics with Selected Sintering Additives[J].Biomaterials,1997,18(13):923.
[2]Moisescu C,Jana C,Rüssel C.Crystallization of Rod-shaped Fluoroapatite from Glass Melts in the System SiO2-Al2O3-CaO-P2O5-Na2O-K2O-F[J].Journal of Non-Crystalline Solids,1999,248(248):169-175.
[3]H9land W,Rheinberger V,Wegner S,et al.Needle-like Apatite-leucite Glass-ceramic as a Base Material for the Veneering of Metal Restorations in Dentistry[J].Journal of Materials Science Materials in Medicine,2000,11(1):11-17.
[4]O'Flynn K P,Stanton K T.Controlling the Crystallization of Fluorapatite in Apatite-Mullite Glass-Ceramics[J].Crystal Growth&Design,2012,12(3):1218-1226.
[5]Chen J,Yan B,Li H,et al.Vitrification of Blast Furnace Slag and Fluorite Tailings for Giving Diopside-fluorapatite Glass-ceramics[J].Materials Letters,2018,218(1):309-312.
[6]张彦辉,亢静锐,李龙梅.氟磷灰石微晶玻璃的烧结与性能研究[J].山东陶瓷,2016,39(10):3-6.
[7]亢静锐,赵亚彬,侯锁霞,等.氟磷灰石生物微晶玻璃的制备与性能[J].材料科学与工程学报,2016,34(1):156-159.
[8]赵英娜,侯锁霞,亢静锐,等.Na2O-B2O3-SiO2-CaO-P2O5-F生物微晶玻璃制备与性能研究[J].人工晶体学报,2016,45(6):1559-1663.
[9]Kokubo T,Kushitani H,Sakka S,et al.Solutions Able to Reproduce in Vivo Surface-structure Changes in Bioactive Glass-ceramic A-W[J].JBiomed Mater Res,1990,24(6):721-734.
[10]Siriphannon P,Kameshima Y,Yasumori A,et al.Comparitive Study of the Formation of Hydroxyapatite in Simulated Body Fluid under Static and Flowing Systems[J].Journal of Biomedical Materials Research Part A,2002,60(1):175-185.
[11]姚树玉,王士栋,周宁,等.烧结法制备粉煤灰微晶玻璃[J].金属热处理,2010,35(4):18-20.
[12]姚树玉,王宗峰,韩野,等.粉煤灰制备透辉石微晶玻璃及其结构分析[J].材料热处理学报,2013,34(7):22-26.
[13]仲维卓,华素坤.晶体生长形态学[M].北京:科学出版社,1999.
[14]H9land W,Ritzberger C,Apel E,et al.Formation and Crystal Growth of Needle-like Fluoroapatite in Functional Glass-ceramics[J].Journal of Materials Chemistry,2008,18(12):1318-1332.
[15]Kokubo T,Takadama H.How Useful is SBF in Predicting in Vivo Bone Bioactivity[J].Biomaterials,2006,27(15):2907-2915.
[16]Suchanek W,Yashima M,Kakihana M,et al.Hydroxyapatite Ceramics with Selected Sintering Additives[J].Biomaterials,1997,18(13):923-933.
[17]Bohner M,Lemaitre J.Can Bioactivity be Tested in Vitro with SBF Solution[J].Biomaterials,2009,30(12):2175-2179.
[18]Ghosh S,Dandapat N,Balla V K.Preparation and in Vitro,Characterization of Fluroapatite Based Bioactive Glass-ceramics for Biomedical Applications[J].Materials Today Proceedings,2015,2(4-5):1326-1331.
[19]Cho S H,Joo S M,Cho J S,et al.Ceramic Processing Research Mechanical Properties and Workability of Self-hardening Calcium Phosphate cement as a Function of the Particle Size Distribution[J].Journal of Ceramic Processing Research,2005,6(1):57-62.
[20]Jmal N,Bouaziz J.Synthesis,Characterization and Bioactivity of a Calcium-phosphate Glass-ceramics Obtained by the Sol-gel Processing Method[J].Materials Science&Engineering C,2017(71):279-288.
[2]Moisescu C,Jana C,Rüssel C.Crystallization of Rod-shaped Fluoroapatite from Glass Melts in the System SiO2-Al2O3-CaO-P2O5-Na2O-K2O-F[J].Journal of Non-Crystalline Solids,1999,248(248):169-175.
[3]H9land W,Rheinberger V,Wegner S,et al.Needle-like Apatite-leucite Glass-ceramic as a Base Material for the Veneering of Metal Restorations in Dentistry[J].Journal of Materials Science Materials in Medicine,2000,11(1):11-17.
[4]O'Flynn K P,Stanton K T.Controlling the Crystallization of Fluorapatite in Apatite-Mullite Glass-Ceramics[J].Crystal Growth&Design,2012,12(3):1218-1226.
[5]Chen J,Yan B,Li H,et al.Vitrification of Blast Furnace Slag and Fluorite Tailings for Giving Diopside-fluorapatite Glass-ceramics[J].Materials Letters,2018,218(1):309-312.
[6]张彦辉,亢静锐,李龙梅.氟磷灰石微晶玻璃的烧结与性能研究[J].山东陶瓷,2016,39(10):3-6.
[7]亢静锐,赵亚彬,侯锁霞,等.氟磷灰石生物微晶玻璃的制备与性能[J].材料科学与工程学报,2016,34(1):156-159.
[8]赵英娜,侯锁霞,亢静锐,等.Na2O-B2O3-SiO2-CaO-P2O5-F生物微晶玻璃制备与性能研究[J].人工晶体学报,2016,45(6):1559-1663.
[9]Kokubo T,Kushitani H,Sakka S,et al.Solutions Able to Reproduce in Vivo Surface-structure Changes in Bioactive Glass-ceramic A-W[J].JBiomed Mater Res,1990,24(6):721-734.
[10]Siriphannon P,Kameshima Y,Yasumori A,et al.Comparitive Study of the Formation of Hydroxyapatite in Simulated Body Fluid under Static and Flowing Systems[J].Journal of Biomedical Materials Research Part A,2002,60(1):175-185.
[11]姚树玉,王士栋,周宁,等.烧结法制备粉煤灰微晶玻璃[J].金属热处理,2010,35(4):18-20.
[12]姚树玉,王宗峰,韩野,等.粉煤灰制备透辉石微晶玻璃及其结构分析[J].材料热处理学报,2013,34(7):22-26.
[13]仲维卓,华素坤.晶体生长形态学[M].北京:科学出版社,1999.
[14]H9land W,Ritzberger C,Apel E,et al.Formation and Crystal Growth of Needle-like Fluoroapatite in Functional Glass-ceramics[J].Journal of Materials Chemistry,2008,18(12):1318-1332.
[15]Kokubo T,Takadama H.How Useful is SBF in Predicting in Vivo Bone Bioactivity[J].Biomaterials,2006,27(15):2907-2915.
[16]Suchanek W,Yashima M,Kakihana M,et al.Hydroxyapatite Ceramics with Selected Sintering Additives[J].Biomaterials,1997,18(13):923-933.
[17]Bohner M,Lemaitre J.Can Bioactivity be Tested in Vitro with SBF Solution[J].Biomaterials,2009,30(12):2175-2179.
[18]Ghosh S,Dandapat N,Balla V K.Preparation and in Vitro,Characterization of Fluroapatite Based Bioactive Glass-ceramics for Biomedical Applications[J].Materials Today Proceedings,2015,2(4-5):1326-1331.
[19]Cho S H,Joo S M,Cho J S,et al.Ceramic Processing Research Mechanical Properties and Workability of Self-hardening Calcium Phosphate cement as a Function of the Particle Size Distribution[J].Journal of Ceramic Processing Research,2005,6(1):57-62.
[20]Jmal N,Bouaziz J.Synthesis,Characterization and Bioactivity of a Calcium-phosphate Glass-ceramics Obtained by the Sol-gel Processing Method[J].Materials Science&Engineering C,2017(71):279-288.