CN108042852A - 一种压电陶瓷/骨水泥生物压电复合材料的制备方法 - Google Patents

一种压电陶瓷/骨水泥生物压电复合材料的制备方法 Download PDF

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CN108042852A
CN108042852A CN201711162174.8A CN201711162174A CN108042852A CN 108042852 A CN108042852 A CN 108042852A CN 201711162174 A CN201711162174 A CN 201711162174A CN 108042852 A CN108042852 A CN 108042852A
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汤玉斐
段子豪
赵康
吴聪
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Abstract

本发明公开了一种压电陶瓷/骨水泥生物压电复合材料的制备方法,包括以下步骤:步骤1,制备压电多孔支架;步骤2,制备磷酸钙骨水泥前驱体:步骤3,制备生物压电复合材料预制体;步骤4,自固化及极化,最后制备得到压电陶瓷/骨水泥生物压电复合材料。本发明方法解决了目前生物压电材料压电相含量过高,细胞生长过程中骨传导性差;采用传统物理共混降低压电相含量,压电系数低起不到骨诱导效果;以及羟基磷灰石和生物压电陶瓷共同烧结无法达到材料性能最优的问题。

Description

一种压电陶瓷/骨水泥生物压电复合材料的制备方法
技术领域
本发明涉及生物医用材料制备方法技术领域,具体涉及一种压电陶瓷/骨水泥生物压电复合材料的制备方法。
背景技术
每年由于疾病或者是交通事故,在世界各地有数百万的患者需要接受骨移植手术,因此促生了骨替代材料的研究和发展。骨替代材料由仿骨基质成分合成,都具有较好的生物相容性,不仅能够与周围受体骨组织良好融合,同时某些人工骨材料能稳定降解。此外人工骨材料最大的优势在于其自身成分、性能能任意调节,不仅能保留良好的生物相容性又无任何免疫反应。骨替代材料多由钙磷盐类物质组成,其虽存在骨传导性能使细胞粘附生长却不能诱导成骨细胞的生长;通过对人骨的研究表明,人体的骨组织是一种天然的压电材料,在受力时骨会产生电信号进而刺激细胞的增殖和分化。因此将压电材料引入这类骨替代材料中便会使得该材料在具有骨传导性的同时,兼顾骨诱导性。目前研究较多的是钛酸钡/羟基磷灰石复合材料,但由于这类材料仅仅通过物理共混复合,压电材料颗粒只有含量很高时才能相互连接,从而达到适合的压电系数,这使得羟基磷灰石含量很少,导致骨传导性丧失很多;但若减少压电颗粒的含量则会让压电相相互孤立,导致材料整体的压电系数很低,达不到刺激细胞增殖分化的目的;同时在复合材料制备过程中基本都是将钛酸钡和羟基磷灰石共混后烧结,但钛酸钡的最佳烧结温度为1300℃,羟基磷灰石烧结温度在1200℃左右,由于两种物质的最佳烧结温度相差很大,使用同一温度烧结会让材料无法达到性能最佳。因此寻找一种仅降低压电相含量但同时让材料具有合适的压电系数,并且避免将钛酸钡和羟基磷灰石同时烧结,保证其两者性能最优是生物压电骨替代材料的难点和重点。
专利《压电型磷酸钙骨水泥复合材料》(申请号:CN201110435435.5,公开日:2012-04-25,公开号:CN102423504A)公开了一种骨水泥固相粉末,采用磷酸钙骨水泥粉末和纳米压电粉混合,加入液相固化的方法制得。该方法让压电颗粒分散在基体骨水泥中,无法实现压电颗粒的相互连接因此压电系数很低,达不到刺激细胞增殖分化的目的。
硕士论文《BaTiO3/PMMA压电复合材料及其极化研究》(2005年四川大学硕士论文)使用义齿基托材料PMMA和钛酸钡复合制备压电材料,由于该材料制备也是采用物理共混的方式去完成,因此只有当钛酸钡含量高于80%时才能保证钛酸钡颗粒之间有相互连接,得到合适的压电系数。
文献《Improved osteoblasts growth on osteomimetic Hydroxyapatite/BaTiO3composites with aligned lamellar porous structure》(2016年《MaterialsScience and Engineering C》第61期8-14页)通过冰模板法制备了孔隙率为40%,50%和60%的多孔羟基磷灰石(HA)/钛酸钡(BaTiO3)压电复合材料。但是该材料中压电相BaTiO3含量高达90%,钛酸钡在体内不会被降解因此大量的BaTiO3残存会对人体造成伤害;另外在其制备过程中将HA和BaTiO3同时进行1250℃高温烧结,由于两种物质的最佳烧结温度相差较大,这样烧制出的材料会对材料力学性能、压电系数产生影响。
专利《一种功能仿生复合生物压电陶瓷材料及其制备方法》(申请号:CN201510100764.2,公开日:2015-07-08,公开号:CN104761253A)公开一种将稀土掺杂压电陶瓷粉料和稀土掺杂生物陶瓷粉料混合,经成型、烧结、极化得到的生物压电陶瓷材料的制备工艺。其中压电相含量大于50%,由于压电颗粒含量少,压电陶瓷颗粒相互独立,使得整体材料压电系数在5pC/N以下,促进细胞的增殖能力有限。
发明内容
本发明的目的是提供一种压电陶瓷/骨水泥生物压电复合材料的制备方法,解决了目前生物压电材料压电相含量过高,细胞生长过程中骨传导性差的问题。
本发明所采用的技术方案是,一种压电陶瓷/骨水泥生物压电复合材料的制备方法,包括以下步骤:
1.一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,包括以下步骤:
步骤1,制备压电多孔支架:
步骤1.1,按照体积百分比称取以下组分:压电陶瓷粉末10%~30%,分散剂1%~2%,粘结剂0.8%~1%,蒸馏水67%~88.2%,上述各组分体积百分比之和为100%;
步骤1.2,将步骤1.1称取的各组分混合均匀,真空除气泡,注入模具中,在-75℃下冷冻2小时后,真空干燥48小时,最终在1300℃温度下烧结2小时得到压电多孔支架;
步骤2,制备磷酸钙骨水泥前驱体:
步骤2.1,按照质量百分比称取以下组分:磷酸氢钙30%~35%,磷酸四钙65%~70%,上述组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥固相;
步骤2.2,按照质量百分比称取以下组分:由步骤2.1制备得到的磷酸钙骨水泥固相64%~67%,骨水泥液相33%~36%,上述各组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥前驱体;
步骤3,制备生物压电复合材料预制体:
步骤3.1,按照体积百分比称取以下组分:由步骤1.2制备得到的压电多孔支架30%~55%,由步骤2.2制备得到的磷酸钙骨水泥前驱体45%~70%,上述组分体积百分比之和为100%;
步骤3.2,将磷酸钙骨水泥前驱体填充到压电多孔支架中,得到生物压电磷酸钙骨水泥预制体;
步骤4:自固化及极化:
将步骤3.2得到的生物压电复合材料预制体放入湿度为100%,温度为37℃的环境中固化48h,并在介质中进行极化处理即可得到一种压电陶瓷/骨水泥生物压电复合材料。
本发明的特点还在于,
步骤1.1中,压电陶瓷粉末为钛酸钡、钛酸钙、铌酸锂钠钾、铌酸钾钠、钛酸铋钠、锆钛酸钡钙中的任意一种;分散剂为十二烷基苯磺酸钠、聚丙烯酸钠、柠檬酸、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;粘结剂为聚乙烯醇、聚乙烯吡咯烷酮、羧甲基纤维素、阿拉伯树胶中的一种。
步骤3.2中,采用拉浸渍法将磷酸钙骨水泥前驱体填充到压电多孔支架中;拉浸渍法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将制得的压电多孔支架置入磷酸钙骨水泥前驱体中浸渍5min,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复4~7次。
步骤3.2中,采用注入法将磷酸钙骨水泥前驱体填充到压电多孔支架中;注入法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将磷酸钙骨水泥前驱体按照1mm/min的注射速度注入压电多孔支架中,当压电多孔支架完全被磷酸钙骨水泥填充后,停止注射。
步骤2.2中,骨水泥液相为蒸馏水、血液、生理盐水、稀酸、血清、磷酸盐溶液中的任意一种。
步骤4中的介质为空气、有机硅油中的任意一种,极化条件为:极化电压1kV~4kV,极化温度为60℃~120℃,极化时间为30min~60min。
本发明的有益效果为:本发明方法解决了目前生物压电材料压电相含量过高,细胞生长过程中骨传导性差;采用传统物理共混降低压电相含量,压电系数低起不到骨诱导效果;以及羟基磷灰石和生物压电陶瓷共同烧结无法达到材料性能最优的问题。
附图说明
图1是应用本发明方法制备得到的压电陶瓷/骨水泥生物压电复合材料垂直于冷冻方向的截面示意图;
图2是应用本发明方法制备得到的压电陶瓷/骨水泥生物压电复合材料平行于冷冻方向的截面示意图。
图中,1.压电多孔支架,2.磷酸钙骨水泥。
具体实施方式
下面结合附图及具体实施方式对本发明进行详细说明。
本发明的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,包括以下步骤:
步骤1,制备压电多孔支架:
步骤1.1,按照体积百分比称取以下组分:压电陶瓷粉末10%~30%,分散剂1%~2%,粘结剂0.8%~1%,蒸馏水67%~88.2%,上述各组分体积百分比之和为100%;
步骤1.1中,所述压电陶瓷粉末为钛酸钡、钛酸钙、铌酸锂钠钾、铌酸钾钠、钛酸铋钠、锆钛酸钡钙中的任意一种;所述分散剂为十二烷基苯磺酸钠、聚丙烯酸钠、柠檬酸、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;所述粘结剂为聚乙烯醇、聚乙烯吡咯烷酮、羧甲基纤维素、阿拉伯树胶中的一种;
步骤1.2,将步骤1.1称取的各组分混合均匀,真空除气泡,注入模具中,在-75℃下冷冻2小时后,真空干燥48小时,最终在1300℃温度下烧结2小时得到压电多孔支架;
步骤2,制备磷酸钙骨水泥前驱体:
步骤2.1,按照质量百分比称取以下组分:磷酸氢钙30%~35%,磷酸四钙65%~70%,上述组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥固相;
步骤2.2,按照质量百分比称取以下组分:由步骤2.1制备得到的磷酸钙骨水泥固相64%~67%,骨水泥液相33%~36%,上述各组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥前驱体;
步骤2.2中,骨水泥液相为蒸馏水、血液、生理盐水、稀酸、血清、磷酸盐溶液中的任意一种;
步骤3,制备生物压电复合材料预制体:
步骤3.1,按照体积百分比称取以下组分:由步骤1.2制备得到的压电多孔支架30%~55%,由步骤2.2制备得到的磷酸钙骨水泥前驱体45%~70%,上述组分体积百分比之和为100%;
步骤3.2,将磷酸钙骨水泥前驱体填充到压电多孔支架中,得到生物压电磷酸钙骨水泥预制体;
步骤3.2中,采用拉浸渍法将磷酸钙骨水泥前驱体填充到压电多孔支架中;拉浸渍法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将制得的压电多孔支架置入磷酸钙骨水泥前驱体中浸渍5min,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复4~7次;
步骤3.2中,采用注入法将磷酸钙骨水泥前驱体填充到压电多孔支架中;注入法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将磷酸钙骨水泥前驱体按照1mm/min的注射速度注入压电多孔支架中,当压电多孔支架完全被磷酸钙骨水泥填充后,停止注射;
步骤4:自固化及极化:
将步骤3.2得到的生物压电复合材料预制体放入湿度为100%,温度为37℃的环境中固化48h,并在介质中进行极化处理即可得到一种压电陶瓷/骨水泥生物压电复合材料;
步骤4中的介质为空气、有机硅油中的任意一种,极化条件为:极化电压1kV~4kV,极化温度为60℃~120℃,极化时间为30min~60min。
图1是应用本发明方法制备得到的压电陶瓷/骨水泥生物压电复合材料垂直于冷冻方向的截面示意图,从图1中可以看出,磷酸钙骨水泥2完全注入压电多孔支架1中,磷酸钙骨水泥2和压电多孔支架1间隔排列;
图2是应用本发明方法制备得到的压电陶瓷/骨水泥生物压电复合材料平行于冷冻方向的截面示意图,从图2中可以看出,磷酸钙骨水泥2在压电多孔支架1中填充良好,通过冷冻干燥法制备的压电多孔支架1上下贯通,保证了压电颗粒相互连接。
实施例1
步骤1:制备压电多孔支架
按照体积百分比分别取钛酸钡粉末10%,十二烷基苯磺酸钠1%,聚乙烯醇0.8%,蒸馏水88.2%,上述各组分体积百分比为100%,将上述的成分混合均匀,在真空环境去除气泡后,注入模具中,在-75℃下冷冻2小时后,在真空环境下干燥48小时,最终在1300℃温度下烧结2小时得到体积分数为30%的压电多孔支架;
步骤2:制备磷酸钙骨水泥前驱体
按照质量百分比取磷酸氢钙30%,磷酸四钙70%,上述组分质量百分比之和为100%,混合均匀,得到磷酸钙骨水泥固相;按照质量百分比取磷酸钙骨水泥固相64%,磷酸盐溶液36%,上述各组分质量百分比之和为100%,将磷酸钙骨水泥固相和骨水泥液相混合均匀,得到磷酸钙骨水泥前驱体;
步骤3:制备生物压电复合材料预制体
取步骤1得到的体积分数为30%的压电多孔支架,按照体积百分比取步骤2得到的磷酸钙骨水泥前驱体70%,上述组分体积百分比之和为100%,将磷酸钙骨水泥前驱体通过在配完磷酸钙骨水泥前驱体5min后并于23min前,将制得的压电多孔支架置入骨水泥前驱体中浸渍5分钟,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复7次,得到生物压电磷酸钙骨水泥预制体;
步骤4:自固化及极化
将步骤3得到的生物压电复合材料预制体体放入湿度为100%,温度为37℃的环境中固化48h,并在有机硅油中,按照4kV的极化电压,60℃的极化温度,极化30min,即得到具有压电多孔支架的组织工程人工骨材料。
实施例2
步骤1:制备压电多孔支架
按照体积百分比分别取铌酸钾钠粉末30%,柠檬酸2%,聚乙烯吡咯烷酮1%,蒸馏水67%,上述各组分体积百分比为100%,将上述的成分混合均匀,在真空环境去除气泡后,注入模具中,在-75℃下冷冻2小时后,在真空环境下干燥48小时,最终在1300℃温度下烧结2小时得到体积分数为55%的压电多孔支架;
步骤2:制备磷酸钙骨水泥前驱体
按照质量百分比取磷酸氢钙35%,磷酸四钙65%,上述组分质量百分比之和为100%,混合均匀,得到磷酸钙骨水泥固相;按照质量百分比取磷酸钙骨水泥固相67%,蒸馏水33%,上述各组分质量百分比之和为100%,将磷酸钙骨水泥固相和骨水泥液相混合均匀,得到磷酸钙骨水泥前驱体;
步骤3:制备生物压电复合材料预制体
取步骤1得到的体积分数为55%的压电多孔支架,按照体积百分比取步骤2得到的磷酸钙骨水泥前驱体45%,上述组分体积百分比之和为100%,在配完磷酸钙骨水泥前驱体7min后并于18min前,将磷酸钙骨水泥前驱体按照1mm/min的注射速度注入压电多孔支架中,当多孔支架完全被磷酸钙骨水泥填充后,停止注射;
步骤4:自固化及极化
将步骤3得到的生物压电复合材料预制体体放入湿度为100%,温度为37℃的环境中固化48h,并在空气介质中在1kV的极化电压,极化温度为120℃下,极化60min,即得到具有压电多孔支架的组织工程人工骨材料。
实施例3
步骤1:制备压电多孔支架
按照体积百分比分别取压钛酸铋钠粉末15%,聚丙烯酸钠1%,羧甲基纤维素1%,蒸馏水83%,上述各组分体积百分比为100%,将上述的成分混合均匀,在真空环境去除气泡后,注入模具中,在-75℃下冷冻2小时后,在真空环境下干燥48小时,最终在1300℃温度下烧结2小时得到体积分数为33%的压电多孔支架;
步骤2:制备磷酸钙骨水泥前驱体
按照质量百分比取磷酸氢钙32%,磷酸四钙68%,上述组分质量百分比之和为100%,混合均匀,得到磷酸钙骨水泥固相;按照质量百分比取磷酸钙骨水泥固相65%,骨水泥液相35%,上述各组分质量百分比之和为100%,将磷酸钙骨水泥固相和骨水泥液相混合均匀,得到磷酸钙骨水泥前驱体;
步骤3:制备生物压电复合材料预制体
取步骤1得到的体积分数为33%的压电多孔支架,按照体积百分比取步骤2得到的磷酸钙骨水泥前驱体67%,上述组分体积百分比之和为100%,在配完磷酸钙骨水泥前驱体6min后,20min前,将制得的压电多孔支架置入骨水泥前驱体中浸渍5分钟,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复5次;
步骤4:自固化及极化
将步骤3得到的生物压电复合材料预制体体放入湿度为100%,温度为37℃的环境中固化48h,并在有机硅油中,按照3kV的极化电压,100℃的极化温度,极化35min,即得到具有压电多孔支架的组织工程人工骨材料。
实施例4
步骤1:制备压电多孔支架
按照体积百分比分别取钛酸钡粉末20%,聚甲基丙烯酸2%,阿拉伯树胶1%,蒸馏水77%,上述各组分体积百分比为100%,将上述的成分混合均匀,在真空环境去除气泡后,注入模具中,在-75℃下冷冻2小时后,在真空环境下干燥48小时,最终在1300℃温度下烧结2小时得到体积分数为38%的压电多孔支架;
步骤2:制备磷酸钙骨水泥前驱体
按照质量百分比取磷酸氢钙30%,磷酸四钙70%,上述组分质量百分比之和为100%,混合均匀,得到磷酸钙骨水泥固相;按照质量百分比取磷酸钙骨水泥固相67%,骨水泥液相33%,上述各组分质量百分比之和为100%,将磷酸钙骨水泥固相和骨水泥液相混合均匀,得到磷酸钙骨水泥前驱体;
步骤3:制备生物压电复合材料预制体
取步骤1得到的体积分数为38%的压电多孔支架,按照体积百分比取步骤2得到的磷酸钙骨水泥前驱体62%,上述组分体积百分比之和为100%,在配完磷酸钙骨水泥前驱体5min后并于23min前,将磷酸钙骨水泥前驱体按照1mm/min的注射速度注入压电多孔支架中,当多孔支架完全被磷酸钙骨水泥填充后,停止注射;
步骤4:自固化及极化
将步骤3得到的生物压电复合材料预制体体放入湿度为100%,温度为37℃的环境中固化48h,并在有机硅油中,按照3kV的极化电压,90℃的极化温度,极化30min,即得到具有压电多孔支架的组织工程人工骨材料。
实施例5
步骤1:制备压电多孔支架
按照体积百分比分别取钛酸钡粉末25%,十二烷基苯磺酸钠1.5%,聚乙烯醇0.5%,蒸馏水73%,上述各组分体积百分比为100%,将上述的成分混合均匀,在真空环境去除气泡后,注入模具中,在-75℃下冷冻2小时后,在真空环境下干燥48小时,最终在1300℃温度下烧结2小时得到体积分数为30%的压电多孔支架;
步骤2:制备磷酸钙骨水泥前驱体
按照质量百分比取磷酸氢钙30%,磷酸四钙70%,上述组分质量百分比之和为100%,混合均匀,得到磷酸钙骨水泥固相;按照质量百分比取磷酸钙骨水泥固相64%,磷酸盐溶液36%,上述各组分质量百分比之和为100%,将磷酸钙骨水泥固相和骨水泥液相混合均匀,得到磷酸钙骨水泥前驱体;
步骤3:制备生物压电复合材料预制体
取步骤1得到的体积分数为40%的压电多孔支架,按照体积百分比取步骤2得到的磷酸钙骨水泥前驱体60%,上述组分体积百分比之和为100%,将磷酸钙骨水泥前驱体通过在配完磷酸钙骨水泥前驱体5min后并于23min前,将制得的压电多孔支架置入骨水泥前驱体中浸渍5分钟,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复7次,得到生物压电磷酸钙骨水泥预制体;
步骤4:自固化及极化
将步骤3得到的生物压电复合材料预制体体放入湿度为100%,温度为37℃的环境中固化48h,并在有机硅油中,按照4kV的极化电压,60℃的极化温度,极化30min,即得到具有压电多孔支架的组织工程人工骨材料。
本发明实施例1、2、3、4、5制备的一种压电陶瓷/骨水泥生物压电复合材料和通过物理共混制得的压电骨水泥的抗压强度、不可降解压电相含量、压电系数的比较如下表所示:
由上表可以看出,由于对压电相颗粒进行了单独烧结,使得所得低压电相的骨替代材料的抗压强度明显大于采用物理共混制得的生物压电材料;与此同时这种压电多孔支架的存在,也保证了压电颗粒的相互连接,使得材料即使只有较低的压电相体积分数仍然有比物理共混更高的压电系数。
本发明的制备方法有如下优点:本发明方法中使用冷冻干燥法制备压电多孔支架,保证压电颗粒相互连接。当材料受到外加载荷作用后,压电颗粒受力产生电荷,电荷在相互连接的颗粒中传播并叠加,从而使得骨替代材料在较低的压电相含量的情况下,仍然具备有较高的压电系数;另一方面通过对压电多孔支架的单独烧结,能让压电材料的性能达到最优,使其具有更高的压电系数,更好的力学性能,并且避免了羟基磷灰石和压电多孔支架烧结温度不一致的问题,磷酸钙骨水泥是一种无需烧结,经自固化便可生成羟基磷灰石的骨替代材料,通过提拉浸渍法和注入法利用其优良的流动性便可填充满整个支架中的孔隙;低的压电相含量也相对提高了骨水泥的含量使得材料最终含有更多的羟基磷灰石,促进了整个材料的骨传导性。

Claims (6)

1.一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,包括以下步骤:
步骤1,制备压电多孔支架:
步骤1.1,按照体积百分比称取以下组分:压电陶瓷粉末10%~30%,分散剂1%~2%,粘结剂0.8%~1%,蒸馏水67%~88.2%,上述各组分体积百分比之和为100%;
步骤1.2,将步骤1.1称取的各组分混合均匀,真空除气泡,注入模具中,在-75℃下冷冻2小时后,真空干燥48小时,最终在1300℃温度下烧结2小时得到压电多孔支架;
步骤2,制备磷酸钙骨水泥前驱体:
步骤2.1,按照质量百分比称取以下组分:磷酸氢钙30%~35%,磷酸四钙65%~70%,上述组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥固相;
步骤2.2,按照质量百分比称取以下组分:由步骤2.1制备得到的磷酸钙骨水泥固相64%~67%,骨水泥液相33%~36%,上述各组分质量百分比之和为100%,将上述组分混合均匀,得到磷酸钙骨水泥前驱体;
步骤3,制备生物压电复合材料预制体:
步骤3.1,按照体积百分比称取以下组分:由步骤1.2制备得到的压电多孔支架30%~55%,由步骤2.2制备得到的磷酸钙骨水泥前驱体45%~70%,上述组分体积百分比之和为100%;
步骤3.2,将磷酸钙骨水泥前驱体填充到压电多孔支架中,得到生物压电磷酸钙骨水泥预制体;
步骤4:自固化及极化:
将步骤3.2得到的生物压电复合材料预制体放入湿度为100%,温度为37℃的环境中固化48h,并在介质中进行极化处理即可得到一种压电陶瓷/骨水泥生物压电复合材料。
2.根据权利要求1所述的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,步骤1.1中,所述压电陶瓷粉末为钛酸钡、钛酸钙、铌酸锂钠钾、铌酸钾钠、钛酸铋钠、锆钛酸钡钙中的任意一种;所述分散剂为十二烷基苯磺酸钠、聚丙烯酸钠、柠檬酸、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;所述粘结剂为聚乙烯醇、聚乙烯吡咯烷酮、羧甲基纤维素、阿拉伯树胶中的一种。
3.根据权利要求1所述的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,步骤3.2中,采用拉浸渍法将磷酸钙骨水泥前驱体填充到压电多孔支架中;拉浸渍法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将制得的压电多孔支架置入磷酸钙骨水泥前驱体中浸渍5min,再缓慢提拉出压电多孔支架,于37℃下静置30分钟,该步骤重复4~7次。
4.根据权利要求1所述的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,步骤3.2中,采用注入法将磷酸钙骨水泥前驱体填充到压电多孔支架中;注入法的具体实施过程为:在配完磷酸钙骨水泥前驱体5min~23min内,将磷酸钙骨水泥前驱体按照1mm/min的注射速度注入压电多孔支架中,当压电多孔支架完全被磷酸钙骨水泥填充后,停止注射。
5.根据权利要求1所述的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,步骤2.2中,骨水泥液相为蒸馏水、血液、生理盐水、稀酸、血清、磷酸盐溶液中的任意一种。
6.根据权利要求1所述的一种压电陶瓷/骨水泥生物压电复合材料的制备方法,其特征在于,步骤4中的介质为空气、有机硅油中的任意一种,极化条件为:极化电压1kV~4kV,极化温度为60℃~120℃,极化时间为30min~60min。
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