尿素添加量对水浴合成羟基磷灰石晶须组成、形貌和结构的影响
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摘要
通过不同尿素添加量研究水浴合成法制备羟基磷灰石晶须的过程参数,分析对产物的组成、形貌和结构产生的影响。采用X射线衍射仪(XRD)、红外光谱(FT-IR),扫描电镜(SEM)与能谱(EDS),高分辨率透射显微镜(HRTEM)等分析手段,对HA晶须的相结构、化学基团、微区成分和微观结构进行了表征。结果表明,在水浴条件下,可以成功地合成结晶度高、组成均一的羟基磷灰石晶须。随着尿素量的提高晶须长径比呈现先增加后降低的趋势,在微观形貌上羟基磷灰石晶须逐渐由针状向绒球状转化。通过红外分析,随着尿素的增加,在尿素缓慢分解的过程中,通过二氧化碳和氨的逐步释放,羟基基团、磷酸根基团和碳酸根基团在逐步加强。通过透射电子显微镜的分析,可以证明晶须沿c轴方向生长,恰当控制尿素的量,可以调控晶须的长径比,也可以通过尿素量的调控,获得一种绒球状羟基磷灰石粉体。
The effects of different urea additions on the composition,morphology and structure of water bath synthesized hydroxyapatite whiskers( HAw) were investigated via X-ray diffraction( XRD),Fourier Transformation Infrared Spectroscopy( FT-IR),scanning electron microscopy( SEM) as well as Energy Dispersive Spectroscopy( EDS) and High Resolution Transmission Electron Microscopy( HRTEM). The phase structure,chemical groups,composition and microstructure of HA whiskers were characterized. It was shown that under hydrothermal conditions,hydroxyapatite whiskers with high crystallinity and uniform composition can be successfully synthesized. As the amount of urea increases,the aspect ratio of whiskers increases at first and then decreases afterword. As to the microscopic morphology,the hydroxyapatite crystals gradually transform from needle like to pellet. Through infrared analysis,the hydroxyl group,the phosphate group and carbonate,with the increase of the amount of urea and the gradual release of carbon dioxide and ammonia, were gradually strengthened. Through the analysis of transmission electron microscopy,it can be proved that the whiskers grow along the c-axis direction,the amount of urea can beproperly controlled so that the aspect ratio of whiskers can be regulated,spheroidal hydroxyapatite powder can be obtained by adjusting the amount of urea added in the batch.
The effects of different urea additions on the composition,morphology and structure of water bath synthesized hydroxyapatite whiskers( HAw) were investigated via X-ray diffraction( XRD),Fourier Transformation Infrared Spectroscopy( FT-IR),scanning electron microscopy( SEM) as well as Energy Dispersive Spectroscopy( EDS) and High Resolution Transmission Electron Microscopy( HRTEM). The phase structure,chemical groups,composition and microstructure of HA whiskers were characterized. It was shown that under hydrothermal conditions,hydroxyapatite whiskers with high crystallinity and uniform composition can be successfully synthesized. As the amount of urea increases,the aspect ratio of whiskers increases at first and then decreases afterword. As to the microscopic morphology,the hydroxyapatite crystals gradually transform from needle like to pellet. Through infrared analysis,the hydroxyl group,the phosphate group and carbonate,with the increase of the amount of urea and the gradual release of carbon dioxide and ammonia, were gradually strengthened. Through the analysis of transmission electron microscopy,it can be proved that the whiskers grow along the c-axis direction,the amount of urea can beproperly controlled so that the aspect ratio of whiskers can be regulated,spheroidal hydroxyapatite powder can be obtained by adjusting the amount of urea added in the batch.
引文
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[4]程宏飞,孙义高,安帅,等.羟基磷灰石的合成及应用研究进展[J].人工晶体学报,2017,46(9):1740-1747.
[5]Yoshio O,Tetsushi I,Toshihiro K,et al.Novel Preparation Method of Hydroxyapatite Fibers[J].Journal of the American Ceramic Society,2010,81(6):1665-1668.
[6]张军,宋邦才,郭进武,等.高长径比羟基磷灰石晶须及其制备方法,CN101148778[P].2008.
[7]汪晓霞,张海黔.羟基磷灰石晶须的水热法合成及表征[J].南京航空航天大学学报,2005,37(5):611-615.
[8]黄志良,罗晶,陈常连,等.压力对均相共沉淀法制备羟基磷灰石晶体形貌的影响[J].武汉工程大学学报,2014(11):43-47.
[9]何前军,黄志良,张联盟,等.羟基磷灰石晶须的控制合成与机理探讨[J].武汉工程大学学报,2005,27(5):36-38.
[10]李剑秋.均相沉淀法制备羟基磷灰石晶须及其台阶生长机理研究[D].武汉:武汉工程大学,2010.
[11]靳治良,李胜利,李武.晶须增强体复合材料的性能与应用[J].盐湖研究,2003,11(4):57-66.
[12]崔永顺.羟基磷灰石晶须材料人工骨支架的制备与性能研究[D].昆明:昆明理工大学,2013.
[13]Neira I S,Guitián F,Taniguchi T,et al.Hydrothermal synthesis of hydroxyapatite whiskers with sharp faceted hexagonal morphology[J].Journal of Materials Science,2008,43(7):2171-2178.
[14]温喜梅,郭进武,张军,等.山梨醇辅助下羟基磷灰石晶须的水热制备[J].无机盐工业,2008,40(11):21-23.
[15]王林,孙清杰,翁履谦,等.纳米羟基磷灰石粉体及其与PEEK复合材料的制备[J].材料开发与应用,2006,21(4):33-37.
[16]王芹,陶杰,汪涛,等.水热法合成羟基磷灰石晶须的工艺研究[J].功能材料,2007(A05):1715-1719.
[17]郭英,李酽,李乐.水热条件下羟基磷灰石纳米晶形成机理[J].中国民航大学学报,2007,25(4):26-30.