CN114751742A - 一种多孔生物压电陶瓷浆料及其支架的制备方法 - Google Patents
一种多孔生物压电陶瓷浆料及其支架的制备方法 Download PDFInfo
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明公开了一种多孔生物压电陶瓷浆料,其包括在水中混合均匀的压电陶瓷粉末、分散剂、粘结剂。本发明还公开了一种多孔生物压电陶瓷支架的制备方法,包括:建模并打印出蜡型支架;处理去除支撑蜡;将多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中,并进行冷冻、真空干燥处理;再进行烧结;最后经过极化处理,即得多孔生物压电陶瓷支架。本发明利用多孔生物压电陶瓷浆料制备多孔生物压电陶瓷支架,该方法利用3D打印技术可打印出结构复杂的支架结构,去除支撑蜡后注入浆料,经过冷冻、干燥、烧结和极化处理后,制备的多孔生物压电陶瓷支架具有孔径可控的三维通孔结构,其结构无污染,具有压电性能、力学性能良好的生物相容性。
Description
技术领域
本发明涉及医用材料技术领域,具体涉及一种多孔生物压电陶瓷浆料,还涉及一种多孔生物压电陶瓷支架的制备方法。
背景技术
科学技术的发展及生活水平的提高使人们更加关注身体健康,这也促进了社会医学技术的快速发展。大量患者身体中硬组织患病或被损坏后可以通过手术进行更换或修复,为了满足医学领域的需求,迫切需要具有优越生物相容性和力学性能的生物医用材料。
目前常规的人工骨支架通常采用具有生物相容性的金属、生物陶瓷、高分子材料及其复合材料制成,但由于金属支架会出现游离金属离子因而存在潜在危险,高分子材料支架的降解产物会导致炎症发生,而陶瓷支架的良好生物相容性为其成为人工骨支架带来巨大优势。
而且,骨组织是天然的压电体,压电效应源于骨的胶原成分,通过机械能和电能的相互转换维持了骨的生理活动和正常的新陈代谢,满足了骨的塑性、改建和功能维持。如果能模拟骨的电活性特征开发具有压电效应的人工骨必将大大提高其生物活性和生物功能性,将压电材料引入骨替代材料中会使材料在具有骨传导性的同时,兼顾骨诱导性,可以赋予骨植入材料与天然骨相类似的生物电活性,通过复合制备手段得到压电性能、力学性能、生物安全和生物相容性都良好的复合仿生骨植入材料。
多孔生物压电陶瓷支架即具有上述优点,目前制备多孔生物压电陶瓷支架的常用方法是添加造孔剂,但该方法无法形成连通孔,甚至会出现空隙封闭。申请号为201910232687.4的中国专利公开了《一种利用冷冻干燥法制备生物压电多孔陶瓷支架的方法》,但此方法只能形成直通孔,并且也无法实现对孔径的可控性。
为了克服现有技术以上问题,本发明提供一种多孔生物压电陶瓷浆料及利用该浆料制备多孔生物压电陶瓷支架的方法。
发明内容
本发明的主要目的在于提供一种多孔生物压电陶瓷浆料。
本发明的主要目的还在于提供一种多孔生物压电陶瓷支架的制备方法,克服了现有的压电陶瓷支架存在的内部结构孔隙不连通的问题。
为实现上述目的,本发明所采用的第一种技术方案是:一种多孔生物压电陶瓷浆料,包括在水中混合均匀的压电陶瓷粉末、分散剂、粘结剂。
作为本发明的另一种实施方式,按照体积分数包括如下组分:压电陶瓷粉末20%~60%,分散剂1%~2%,粘结剂0.8%~1.2%,蒸馏水56.8%~78.2%,上述各组分体积百分比之和为100%。
作为本发明的另一种实施方式,所述压电陶瓷粉末包括铌酸锂钾钠、钛酸钡、钛酸铋钠、锆钛酸钡中的任意一种或至少两种的混合物。
作为本发明的另一种实施方式,所述分散剂包括柠檬酸、聚丙烯酸钠、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;所述粘结剂包括聚乙烯醇、羧甲基纤维素、阿拉伯树胶中的任意一种。
本发明所采用的第二种技术方案是:一种多孔生物压电陶瓷支架的制备方法,包括步骤:
建模并利用3D蜡型打印机打印出具有三维结构的蜡型支架,所述蜡型支架的孔径为400μm至1000μm;
对打印好的所述蜡型支架进行后处理去除支撑蜡;
配置如上所述的多孔生物压电陶瓷浆料;
将所述多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中,并进行冷冻、真空干燥处理;
将经过真空干燥处理的蜡型支架进行烧结,得到多孔生物压电陶瓷支架胚;
对所述多孔生物压电陶瓷支架胚进行极化处理,即得所述多孔生物压电陶瓷支架。
作为本发明的另一种实施方式,所述去除支撑蜡具体是利用乙醇和聚丙二醇的混合溶液清洗所述蜡型支架。
作为本发明的另一种实施方式,将所述多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中具体为:
将所述多孔生物压电陶瓷浆料利用球磨机混合均匀,然后经过真空除气泡后利用真空注型机注入所述蜡型支架中。
作为本发明的另一种实施方式,对所述蜡型支架进行冷冻具体是在-60℃至-80℃下冷冻2至4小时,所述真空干燥时间为24h-48h。
作为本发明的另一种实施方式,将经过真空干燥处理的蜡型支架进行烧结具体为:
在1100℃至1300℃温度下真空烧结2h至3h,自然冷却。
作为本发明的另一种实施方式,对经过烧结得到的多孔生物压电陶瓷支架胚进行极化处理具体为:
将经过烧结的多孔生物压电陶瓷支架胚置于硅油中,极化电场介电强度为3kV/mm至4kV/mm,极化温度为80℃至95℃,极化时间为12min至18min。
与现有技术相比,本发明具有如下有益效果:本发明利用多孔生物压电陶瓷浆料制备一种多孔生物压电陶瓷支架,该方法利用3D打印技术可打印出结构复杂的支架结构,而且可以根据陶瓷零件结构逆向设计模具,不受陶瓷零件自身的复杂形状和结构限制,而且用于凝胶注模的成本较低而坯体和成品强度高、性能好,在去除支撑蜡后注入浆料,经过冷冻、干燥、烧结和极化处理后,利用该方法制备的多孔生物压电陶瓷支架具有孔径可控的三维通孔结构,其结构无污染,具有压电性能、力学性能良好的生物相容性,可广泛用于生物医学和组织工程等领域。
附图说明
图1为本发明多孔生物压电陶瓷支架的制备方法的流程示意图;
图2为本发明制备的多孔生物压电陶瓷支架的内部孔径结构示意图;
图3为本发明实施例1制备的多孔生物压电陶瓷支架的显微组织结构图。
具体实施方式
本发明公开了一种多孔生物压电陶瓷浆料,包括在水中混合均匀的压电陶瓷粉末、分散剂、粘结剂。
本发明通过在水中溶解、稀释压电陶瓷粉末、分散剂和粘结剂,利用分散剂可以使压电陶瓷粉末均匀悬浮、分散于水中,粘结剂则可提高后续烧结处理时的压电陶瓷粉末的强度和防止其偏析,将其制备成浆料供后续制备压电陶瓷支架使用。
具体地,该浆料按照体积分数包括如下组分:压电陶瓷粉末20%~60%,分散剂1%~2%,粘结剂0.8%~1.2%,蒸馏水56.8%~78.2%,上述各组分体积百分比之和为100%。
通过上述组分配比制备的浆料稀稠度、流动性、渗透性合适,可以方便注入去除支撑蜡的蜡型支架中,后续处理后也具有优良的性能。
示例性地,压电陶瓷粉末可以包括铌酸锂钾钠、钛酸钡、钛酸铋钠、锆钛酸钡中的任意一种或至少两种的混合物;分散剂可以选择柠檬酸、聚丙烯酸钠、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;粘结剂可以选择聚乙烯醇、羧甲基纤维素、阿拉伯树胶中的任意一种。
参见图1,本发明还公开一种利用上述多孔生物压电陶瓷浆料制备多孔生物压电陶瓷支架的制备方法,具体包括如下步骤:
建模并利用3D蜡型打印机打印出具有三维结构的蜡型支架,蜡型支架的孔径为400μm至1000μm;
由于人体骨支架结构为非标件,且要求精度高,因此常规铸造工艺难以满足人骨的制造要求,因此本发明利用建模软件进行建模,后利用3D打印出具有三维结构的蜡型支架,3D打印的蜡型支架可以满足人骨结构的要求和制造精度的要求,该蜡型支架的孔径为400μm至1000μm,经过脱蜡后可以注入浆料进行型材铸造,而制备的型材也可以具有三维结构且互相连通的孔隙。示例性地,建模软件可以采用UG、CAD、3DMAX、Solidworks、Zbrush、Maya、Blend、Magics等三维建模软件。3D打印则可以采用3D systems公司的蜡型打印机进行3D打印。
对打印好的蜡型支架进行后处理去除支撑蜡;
示例性地,本实施例去除支撑蜡是利用乙醇和聚丙二醇的混合溶液进行清洗,更具体的,乙醇和聚丙二醇的体积比为3:1。当然,根据蜡型支架中不同支撑蜡的物质特性可以选择不同的后处理方式去除支撑蜡,例如可以采用水浴利用较高水温融化支撑蜡,本发明对此不作详细限定。
配置如上所述的多孔生物压电陶瓷浆料;
将配置好的多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中,并进行冷冻、真空干燥处理;
优选地,将多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中具体为:
先将多孔生物压电陶瓷浆料利用球磨机混合均匀,使得浆料中物料的粒径较细且均匀,而且使得浆料中压电陶瓷粉末分散更加均匀,确保后续处理后的支架结构性能优良,然后经过真空除气泡后利用真空注型机注入蜡型支架中。示例性地,球磨转速可以为300r/min,料球比为10:1,时间设置为24h。
优选地,对该蜡型支架进行冷冻具体是在-60℃至-80℃下冷冻2至4小时,真空干燥时间为24h-48h。经过冷冻和真空干燥后可以确保浆料填充和固定于蜡型支架上,而且去除多余水分。
将经过真空干燥处理的蜡型支架进行烧结得到多孔生物压电陶瓷支架胚;
针对不同的压电陶瓷材料可以选择合适的烧结温度,优选地,本发明的烧结温度为1100℃至1300℃,烧结时间为2h至3h,然后自然冷却。
对经过烧结的多孔生物压电陶瓷支架胚进行极化处理,即得该多孔生物压电陶瓷支架。
在对压电陶瓷结构进行烧结时,需要选择合适的极化电场介电强度、极化温度和极化时间。优选地,本发明对多孔生物压电陶瓷支架胚极化处理具体为:将其置于硅油中,极化电场介电强度为3kV/mm至4kV/mm,极化温度为80℃至95℃,极化时间为12min至18min。
本发明制备得到的多孔生物压电陶瓷支架的内部孔径结构示意图如图2所示,该支架内部具有三维立体连通的通孔,且孔径可控,相比于现有的压电陶瓷支架微观结构无连通孔或者只有直通孔的结构,其具有良好的压电性能,可以模拟骨的电活性特征提高其生物活性和生物功能性,替代骨或促进骨生长、骨愈合,具有非常广阔的应用前景。
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
本实施例提供一种多孔生物压电陶瓷支架的制备方法,包括步骤:
步骤1:使用UG进行三维建模,利用3D systems公司蜡型打印机打印出三维结构的蜡型支架,支架孔径为800μm;
步骤2:将打印好的蜡型进行后处理,用工业酒精和聚丙二醇洗蜡的混合溶液(体积比为3:1),去除支撑蜡;
步骤3:按照体积百分比将铌酸锂钾钠压电陶瓷粉末40%、柠檬酸2%、聚乙烯醇1%和去离子水57%进行混合配成陶瓷浆料;
步骤4:将步骤3制得的铌酸锂钾钠压电陶瓷浆料使用球磨机混合均匀,真空除气泡,使用真空振动注型机,将陶瓷浆料注入三维结构蜡型支架中,在-75℃下冷冻2小时后,真空干燥48小时。
步骤5:在1100℃温度下烧结2小时,除去蜡型,得到多孔生物压电陶瓷支架胚;
步骤6:在硅油中,极化电压3kv,极化温度90℃,极化时间15min,制得多孔生物压电陶瓷支架。
制得的该多孔生物陶瓷支架的显微组织结构图如图3所示,从图3中可知:压电陶瓷的晶粒尺寸均匀,轮廓清晰,呈现出规则的形状,且陶瓷的气孔较少,致密度较高。
实施例2:
本实施例提供一种多孔生物压电陶瓷支架的制备方法,包括步骤:
步骤1:使用3DMAX软件进行三维建模,利用3D systems公司蜡型打印机打印出三维结构的蜡型支架,支架孔径为500μm;
步骤2:将打印好的蜡型进行后处理,用工业酒精和聚丙二醇洗蜡混合配置清洗液(体积比为3:1),去除支撑蜡;
步骤3:按照体积百分比将钛酸钡压电陶瓷粉末50%、聚丙烯酸钠1%、羧甲基纤维素0.8%和去离子水48.2%配成陶瓷浆料;
步骤4:将步骤3配置的钛酸钡压电陶瓷浆料使用球磨机混合均匀,真空除气泡,使用真空注型机,将陶瓷浆料注入三维结构蜡型中,在-75℃下冷冻4小时后,真空干燥48小时;
步骤5:在1300℃温度下烧结2小时,除去蜡型,得到多孔生物压电陶瓷支架胚;
步骤6:在硅油中,极化电压4kv,极化温度90℃,极化时间15min,得到多孔生物压电陶瓷支架。
实施例3:
本实施例提供一种多孔生物压电陶瓷支架的制备方法,包括步骤:
步骤1:使用Solidworks软件进行三维建模,利用3D systems公司蜡型打印机打印出三维结构的蜡型支架,支架孔径在1000μm;
步骤2:将打印好的蜡型进行后处理,用工业酒精和聚丙二醇洗蜡配置清洗液(体积比为3:1),去除支撑蜡;
步骤3:按照体积百分比将锆钛酸钡压电陶瓷粉末40%、聚甲基丙烯酸1%、阿拉伯树胶0.8%和去离子水58.2%配成陶瓷浆料;
步骤4:将步骤3配置的锆钛酸钡压电陶瓷浆料使用球磨机混合均匀,真空除气泡,使用真空注型机,将陶瓷浆料注入三维结构蜡型中,在-75℃下冷冻3小时后,真空干燥30小时;
步骤5:在1200℃温度下烧结2小时,除去蜡型,得到多孔生物压电陶瓷支架胚;
步骤6:在硅油中,极化电压4kv,极化温度90℃,极化时间15min,得到多孔生物压电陶瓷支架。
通过对本发明实施例1、2、3制备的多孔生物压电陶瓷支架以及两个对比例利用常规凝胶注模工艺制备的压电陶瓷支架的压电相含量、压电系数、抗压强度的测量,其数据如下表所示:
由上表可知,相比于常规的制备方法,利用本发明的方法制备的压电陶瓷支架具有较低的压电相含量性能和较高的压电系数,同时还具有较强的抗压强度。
实施例4
本实施例提供一种多孔生物压电陶瓷支架的制备方法,包括步骤:
步骤1:使用UG软件进行三维建模,利用3D systems公司蜡型打印机打印出三维结构的蜡型支架,支架孔径在700μm;
步骤2:将打印好的蜡型进行后处理,用工业酒精和聚丙二醇洗蜡配置清洗液(体积比为3:1),去除支撑蜡;
步骤3:按照体积百分比将锆钛酸钡压电陶瓷粉末20%、钛酸铋钠压电陶瓷粉末20%、聚甲基丙烯酸1%、阿拉伯树胶0.8%和去离子水58.2%配成陶瓷浆料;
步骤4:将步骤3制备的压电陶瓷浆料使用球磨机混合均匀,真空除气泡,使用真空注型机,将陶瓷浆料注入三维结构蜡型中,在-80℃下冷冻2.5小时后,真空干燥24小时;
步骤5:在1150℃温度下烧结2.3小时,除去蜡型,得到多孔生物压电陶瓷支架胚;
步骤6:在硅油中,极化电压3.5kv,极化温度83℃,极化时间17min,得到多孔生物压电陶瓷支架。
实施例4
本实施例提供一种多孔生物压电陶瓷支架的制备方法,包括步骤:
步骤1:使用UG软件进行三维建模,利用3D systems公司蜡型打印机打印出三维结构的蜡型支架,支架孔径在700μm;
步骤2:将打印好的蜡型进行后处理,用工业酒精和聚丙二醇洗蜡配置清洗液(体积比为3:1),去除支撑蜡;
步骤3:按照体积百分比将铌酸锂钾钠压电陶瓷粉末10%、钛酸钡压电陶瓷粉末15%、钛酸铋钠压电陶瓷粉末10%、聚甲基丙烯酸钠1.4%、羧甲基纤维素1%和去离子水62.6%配成多孔生物压电陶瓷浆料;
步骤4:将步骤3制备的多孔生物压电陶瓷浆料使用球磨机混合均匀,真空除气泡,使用真空注型机,将陶瓷浆料注入三维结构蜡型中,在-60℃下冷冻4小时后,真空干燥40小时;
步骤5:在1260℃温度下烧结2.3小时,除去蜡型,得到多孔生物压电陶瓷支架胚;
步骤6:在硅油中,极化电压3.5kv,极化温度92℃,极化时间13min,得到多孔生物压电陶瓷支架。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种多孔生物压电陶瓷浆料,其特征在于,包括在水中混合均匀的压电陶瓷粉末、分散剂、粘结剂。
2.如权利要求1所述的多孔生物压电陶瓷浆料,其特征在于,按照体积分数包括如下组分:压电陶瓷粉末20%~60%,分散剂1%~2%,粘结剂0.8%~1.2%,蒸馏水56.8%~78.2%,上述各组分体积百分比之和为100%。
3.如权利要求1或2所述的多孔生物压电陶瓷浆料,其特征在于,所述压电陶瓷粉末包括铌酸锂钾钠、钛酸钡、钛酸铋钠、锆钛酸钡中的任意一种或至少两种的混合物。
4.如权利要求1或2所述的多孔生物压电陶瓷浆料,其特征在于,所述分散剂包括柠檬酸、聚丙烯酸钠、聚甲基丙烯酸、聚甲基丙烯酸钠中的任意一种;所述粘结剂包括聚乙烯醇、羧甲基纤维素、阿拉伯树胶中的任意一种。
5.一种多孔生物压电陶瓷支架的制备方法,其特征在于,包括步骤:
建模并利用3D蜡型打印机打印出具有三维结构的蜡型支架,所述蜡型支架的孔径为400μm至1000μm;
对打印好的所述蜡型支架进行后处理去除支撑蜡;
配置如权利要求1-4任一项所述的多孔生物压电陶瓷浆料;
将所述多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中,并进行冷冻、真空干燥处理;
将经过真空干燥处理的所述蜡型支架进行烧结,得到多孔生物压电陶瓷支架胚;
对所述多孔生物压电陶瓷支架胚进行极化处理,即得所述多孔生物压电陶瓷支架。
6.如权利要求5所述的多孔生物压电陶瓷支架的制备方法,其特征在于,所述去除支撑蜡具体是利用乙醇和聚丙二醇的混合溶液清洗所述蜡型支架。
7.如权利要求5所述的多孔生物压电陶瓷支架的制备方法,其特征在于,将所述多孔生物压电陶瓷浆料注入去除支撑蜡后的蜡型支架中具体为:
将所述多孔生物压电陶瓷浆料利用球磨机混合均匀,然后经过真空除气泡后利用真空注型机注入所述蜡型支架中。
8.如权利要求5所述的多孔生物压电陶瓷支架的制备方法,其特征在于,对所述蜡型支架进行冷冻具体是在-60℃至-80℃下冷冻2至4小时,所述真空干燥时间为24h-48h。
9.如权利要求5所述的多孔生物压电陶瓷支架的制备方法,其特征在于,将经过真空干燥处理的蜡型支架进行烧结具体为:
在1100℃至1300℃温度下真空烧结2h至3h,然后自然冷却。
10.如权利要求5所述的多孔生物压电陶瓷支架的制备方法,其特征在于,对经过烧结的蜡型支架进行极化处理具体为:
将经过烧结的蜡型支架置于硅油中,极化电场介电强度为3kV/mm至4kV/mm,极化温度为80℃至95℃,极化时间为12min至18min。
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