微波烧结工艺制备纳米羟基磷灰石陶瓷
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摘要
采用微波烧结法对分别以沉淀法和溶胶凝胶法制备技术的羟基磷灰石(HAP)进行烧结,获得了高强度且晶粒可控的HAP陶瓷。利用X射线衍射、场发射扫描电子显微镜、电子万能材料试验机对样品的相组成、微观形貌和力学性能进行了表征。结果表明:以溶胶凝胶法所制备的HAP粉末为原料的陶瓷材料更容易烧结致密;相比无压烧结,微波烧结能够在保证力学性能的基础上降低烧结温度,控制晶粒生长。当以溶胶凝胶法制备的HAP粉末为原料,压制成型,在微波烧结工艺下烧结制度为1 100℃恒温30 min时,可获得弯曲强度为93 MPa、晶粒大小约为300 nm的高强度HAP陶瓷材料。
Two kinds of hydroxyapatite(HAP) materials synthesized by precipitation and sol–gel methods were sintered by a microwave sintering method to obtain high-strength and grain-controllable HAP bioceramics. The phase composition,micro-morphology and mechanical properties of the samples were characterized by X-ray diffraction, field emission scanning electron microscopy and electronic universal material tests. The results show that the HAP powder prepared by sol–gel method is easier to sinter and denser than that by precipitation method. Compared to pressureless sintering, microwave sintering can reduce sintering temperature and make the grains smaller after sintering based on the guaranteeing mechanical properties. When the HAP powder prepared by sol–gel method is pressed and formed, a high-strength HAP ceramic material with a bending strength of 93 MPa and a grain size of approximately 300 nm is obtained, and the sintering system is maintained at 1 100 ℃ for 30 min under microwave sintering.
Two kinds of hydroxyapatite(HAP) materials synthesized by precipitation and sol–gel methods were sintered by a microwave sintering method to obtain high-strength and grain-controllable HAP bioceramics. The phase composition,micro-morphology and mechanical properties of the samples were characterized by X-ray diffraction, field emission scanning electron microscopy and electronic universal material tests. The results show that the HAP powder prepared by sol–gel method is easier to sinter and denser than that by precipitation method. Compared to pressureless sintering, microwave sintering can reduce sintering temperature and make the grains smaller after sintering based on the guaranteeing mechanical properties. When the HAP powder prepared by sol–gel method is pressed and formed, a high-strength HAP ceramic material with a bending strength of 93 MPa and a grain size of approximately 300 nm is obtained, and the sintering system is maintained at 1 100 ℃ for 30 min under microwave sintering.
引文
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[16]李星逸,孟祥才,刘国权,等.烧结工艺对羟基磷灰石组织及性能的影响[J].材料热处理学报,2008,29(6):41-44.LI X Y,MENG X C,LIU G Q,et al.Mater Heat Treat(in Chinese),2008,29(6):41-44.
[17]SUN Q.The effects of sintering temperature on the preparation of HAceramic powder[J].China Ceram,2013,49(2):42-45.
[18]GUO W G,QIU Z Y,CUI H,et al.Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics[J].Front Mater Sci,2013,7(2):190-195.
[19]CHENG Peng,ZHENG Yong,DONG Zuowei,et al.Research Progress in the Preparation Technology of Microwave Dielectric Ceramics[J].Mater Rev,2014,28(1):110-114.
[2]HAN Y J,LI M,LV Y.Research and applications on the hydroxylapatite bio-composites[J].Chem Ind Eng Progr,2004,23(9):968-971.
[3]TANG Jinglong.Research status of the biological safety of nano-hydroxyapatite[J].J Clin Rehab Tissue Eng Res,2007,11(5):936-939+943.
[4]肖镇昆,吴磊,米饶,等.碳纳米管对羟基磷灰石基复合材料力学性能的影响[J].无机化学学报,2015,31(1):114-120.XIAO Zhenkun,WU Lei,MI Rao,et al.J Inorg Chem(in Chinese),2015,31(1):114-120.
[5]孙艳荣,范涛,黄勇,等.羟基磷灰石生物陶瓷材料的研究趋势及展望[J].硅酸盐学报,2010,38(6):1145-1150.SUN Y R,FAN T,HUANG Y,et al.J Chin Ceram Soc,2010,38(6):1145-1150.
[6]LI B,LIAO X,ZHU X,et al.Preparation of porous carbonated hydroxyapatite nanoceramics based on microwave sintering approach[J].J Chin Ceram Soc,2011,39(12):1909-1914.
[7]FANG Z,FENG Q,TAN R.In-situ grown hydroxyapatite whiskers reinforced porous HA bioceramic[J].Ceram Inter,2013,39(8):8847-8852.
[8]LI Yinghua,CAO Liyun,HUANG Jianfeng.Characteristics and preparation of nanometer hydroxyapatite in medical science[J].J Clin Rehab Tissue Eng Res,2008,12(41):8143-8146.
[9]WU Hong,SHI Honggang,FENG Hongwei,et al.Research progress in microwave sintering technology[J].Ord Mater Sci Eng,2004,27(4):59-61.
[10]王念.陶瓷材料的微波烧结特性及应用[J].武汉理工大学学报,2002,24(5):43-46.WANG N.J Wuhan Univ Technol(in Chinese),2002,24(5):43-46.
[11]王飞,周新贵,余金山,等.微波烧结工艺制备陶瓷材料的研究现状[J].材料导报,2011,25(19):28-31.WANG Fei,ZHOU Xingui,YU Jinshan,et al.Mater Rev(in Chinese),2011,25(19):28-31.
[12]王爱娟,吕宇鹏,朱瑞富,等.烧结对羟基磷灰石微球微观形貌和性能的影响[J].材料热处理学报,2007,28(s1):355-358.WANG A J,LV Y P,ZHU R F,et al.T Mater Heat Treat(in Chinese),2007,28(s1):355-358.
[13]WANG J,BINNER J,VAIDHYANATHAN B,et al.Evidence for the microwave effect during hybrid sintering[J].J Am Ceram Soc,2006,89(6):8.
[14]LANDI E,TAMPIERI A,CELOTTI G,et al.Densification behavior and mechanisms of synthetic hydroxyapatites[J].J Eur Ceram Soc,2000,20(14):2377-2387.
[15]AN Y,XU X,GUI K.Effect of SiC whiskers and graphene nanosheets on the mechanical properties of ZrB2-SiCw-graphene ceramic composites[J].Ceram Int,2016,42(12):14066-14070.
[16]李星逸,孟祥才,刘国权,等.烧结工艺对羟基磷灰石组织及性能的影响[J].材料热处理学报,2008,29(6):41-44.LI X Y,MENG X C,LIU G Q,et al.Mater Heat Treat(in Chinese),2008,29(6):41-44.
[17]SUN Q.The effects of sintering temperature on the preparation of HAceramic powder[J].China Ceram,2013,49(2):42-45.
[18]GUO W G,QIU Z Y,CUI H,et al.Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics[J].Front Mater Sci,2013,7(2):190-195.
[19]CHENG Peng,ZHENG Yong,DONG Zuowei,et al.Research Progress in the Preparation Technology of Microwave Dielectric Ceramics[J].Mater Rev,2014,28(1):110-114.