CN116370701A - 一种抗冲击可促成骨分化极小曲面骨支架及其制备方法 - Google Patents
一种抗冲击可促成骨分化极小曲面骨支架及其制备方法 Download PDFInfo
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Abstract
本发明涉及高分子材料技术领域，具体涉及一种抗冲击可促成骨分化极小曲面骨支架及其制备方法，该极小曲面骨支架由ZrO2和Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒混合在特殊的液体中制成的打印材料经纳米粒子喷射3D打印技术打印所得。本发明的极小曲面骨具有较高的静压缩强度以及良好的抗冲击性能，并且能够有效促进成骨细胞的增殖，从而修复骨缺损，从而解决现有骨支架抗冲击性能差的问题，满足生物医学、组织工程等对材料的需求。
Description
技术领域
本发明涉及高分子材料技术领域，具体涉及一种抗冲击可促成骨分化极小曲面骨支架及其制备方法。
背景技术
极小曲面(TPMS)是一类由平均曲率为零的曲面生成的三维多孔结构，具有高比表面积和高承载特性等优异性能，使得TPMS支架在骨组织修复中具有广阔的应用前景。首先，在植入性能方面，TPMS骨支架可以消除应力屏蔽效应的影响，具有很好的承载特性。此外，TPMS结构有更高的压缩强度，并且TPMS相互连通的曲面利于细胞粘附，能够促进细胞的生长。然而目前所研究的TPMS骨支架微观特征尺寸(≥300μm)普遍大于真实骨骼，不能达到模仿真实骨组织尺寸的要求，严重限制了其生物功能的表达。
针对上述关键问题，近年来，一些学者和专家研究了一些具有改进力学性能的骨支架构筑材料和打印方法。传统金属去除支撑材料较为困难，同时由于其生物性能与骨骼不匹配，可能会引起过敏反应和炎症。相比之下，陶瓷硬度远高于高分子材料和金属，特别是氧化锆陶瓷具有良好的生物相容性、高机械强度和良好的化学稳定性。其次，以高分辨率(μm)和高精度(成型误差5％以内)实现超精细结构打印NPJ技术为制备与人体骨骼相似的超精细微型TPMS骨支架提供了可能。
此外，根据人的活动环境和机能极限，骨骼不仅需要承载人体自身重量带来的静压缩载荷，还会受到自身活动引起的频繁的低速冲击载荷。因此，开展骨支架结构相关力学性能研究就非常有必要。但是目前针对可植入TPMS骨支架的承载性能和失效模式的研究不够深入，尤其是对于氧化锆TPMS骨支架的低速冲击性能研究鲜有涉及。
发明内容
为解决上述问题，本发明提供了一种抗冲击可促成骨分化极小曲面骨支架及其制备方法，具有较高的静压缩强度以及良好的抗冲击性能，并且能够有效促进成骨细胞的增殖，从而修复骨缺损，从而解决现有骨支架抗冲击性能差的问题，满足生物医学、组织工程等对材料的需求。
为实现上述目的，本发明采取的技术方案为：
一种抗冲击可促成骨分化极小曲面骨支架，该极小曲面骨支架由ZrO2和Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒混合在特殊的液体中制成的打印材料经纳米粒子喷射3D打印技术打印所得。
进一步地，所述打印材料中，Y2O3、HfO2、Nb2O5、Cao和Al2O3的材料组分分别为4.64％(wt％)、1.47％(wt％)、0.739％(wt％)、0.47％(wt％)和0.38％(wt％)。
进一步地，ZrO2颗粒粒径为100nm-300nm，Y2O3、HfO2和Nb2O5颗粒粒径为50-150nm。
本发明还提供了上述一种抗冲击可促成骨分化极小曲面骨支架的制备方法，包括如下步骤：
S1、根据最有利于骨细胞生长原则，3D建模出常规结构Normal-A以及极小曲面骨支架TPMS-B和极小曲面骨支架TPMS-C；
S2、将ZrO2和Y2O3、HfO2和Nb2O5颗粒按比例混合在特殊的液体中，制成打印材料；
S2、经Carmel 1400打印设备将打印材料准确喷射在打印机托盘相应位置以得到半成品；随后，使用30℃的恒温水槽对半成品进行清洗，然后使用100℃的恒温干燥箱对半成品烘干处理2h，最后利用马弗炉在1200～1500℃下进行无压脱脂烧结，得到精密氧化锆TPMS骨支架成品。
进一步地，所述步骤S1中，Normal-A的孔直径恒定为750μm；TPMS-B的孔径范围设计为200μm～800μm；TPMS-C孔径范围设计为125μm～800μm。
本发明具有以下有益效果：
1)适量加入的Y2O3能够降低氧化锆t相(四方相)的化学自由能，从而抑制其相变，同时促进结构致密度使烧结后的t-ZrO2保持稳定。
2)少量的Nb2O5也能在一定程度上提升氧化锆陶瓷的致密度，还能在不影响结构力学性能的前提下降低烧结温度，在结构制备过程中更容易达到烧结的温度条件。
3)HfO2使t-ZrO2的晶界玻璃相软化，使得结构裂纹钝化和裂纹尖端应力集中削弱，从而提高结构韧性。
4)Normal-A的压缩强度为47.47MPa，压缩模量为1.83GPa。TPMS-B的压缩强度为39.08MPa，压缩模量为2.56GPa，TPMS-C的压缩强度为56.6MPa，压缩模量为2.05GPa，较Normal-A分别提升19.23％和12.02％。
5)Normal-A的冲击应力极限为61.47MPa。TPMS-B的冲击应力极限为44.93MPa。TPMS-C的冲击应力极限为61.47MPa，比Normal-A高14.27％。
6)所得的TPMS骨支架压缩强度高，抗冲击能力强，能够作为骨骼的替代性支架应用于生物医学材料领域。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1为极小曲面骨支架制备原理示意图。
图2为TPMS-B骨支架。
图3为TPMS-C骨支架。
图4为准静态压缩实验结果；
图中：(a)Normal-A应力-应变；(b)TPMS-B应力-应变。
图5为TPMS-B抗冲击试验应力-应变。
图6为(a)TPMS-C准静态压缩试验应力-应变和(b)TPMS-C抗冲击试验应力-应变。
图7为(a)不同Y2O3与HfO2的质量比下TPMS的致密程度，(b)不同Y2O3含量下的TPMS的压缩强度。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1
首先将粒径范围为50～300nm的ZrO2和Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒按浓度要求混合在特殊的液体中，所述特殊的液体购自3D打印机厂商XJET，制成打印材料墨水。然后将设计好的TPMS-B的stl.文件导入Carmel 1400打印设备中，经12288个喷嘴将制成的1.2*108滴墨水准确喷射在打印机托盘相应位置，逐层完成零件的打印，得到半成品，在完成上一层之后，打印平台会降低一层的厚度；将半成品用30℃的恒温水槽清洗以快速去除聚乙烯醇(PVA)水溶性支撑材料后，置于100℃的恒温干燥箱中烘干处理2小时。最后在1300℃的马弗炉内进行无压脱脂烧结，烧结过程中氧化锆晶粒重排，堆积的颗粒会向中心靠近。烧结完成后，氧化锆晶体由单斜晶相(m)转变为四方晶相(t)，得到致密度高达99.5％的精密氧化锆骨支架成品(TPMS-B)。准静态压缩测试表明，极限载荷为39.08MPa，杨氏模量为2.56GPa，模量较Normal-A提升了1.4倍，测试结果如图4。对样品进行了抗冲击试验，结果显示TPMS-B冲击试验的平均强度为44.93MPa，比静力的抗压强度高14.95％，如图5所示。
实施例2
首先将粒径范围为50～300nm的ZrO2和Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒按浓度要求混合在特殊的液体中，制成打印材料墨水。然后将设计好的TPMS-C的stl.文件导入Carmel 1400打印设备中，经12288个喷嘴将制成的1.2*108滴墨水准确喷射在打印机托盘相应位置，逐层完成零件的打印，得到半成品，在完成上一层之后，打印平台会降低一层的厚度；将半成品用30℃的恒温水槽清洗以快速去除聚乙烯醇(PVA)水溶性支撑材料后，置于100℃的恒温干燥箱中烘干处理2小时。最后在1300℃的马弗炉内进行无压脱脂烧结，烧结过程中氧化锆晶粒重排，堆积的颗粒会向中心靠近。烧结完成后，氧化锆晶体由单斜晶相(m)转变为四方晶相(t)，得到致密度高达99.5％的精密氧化锆骨支架成品(TPMS-C)。准静态压缩测试表明，极限载荷为56.6MPa，杨氏模量为2.05GPa，其压缩强度和模量分别比Normal-A高19.23％和12.02％，力学性能最优，并且TPMS-C骨支架2.05GPa的模量与人体松质骨等骨骼模量吻合良好。此外，对样品进行了抗冲击试验，结果显示TPMS-C冲击试验的平均强度为70.23MPa，比静力的抗压强度高24.09％，表明本专利描述的TPMS-C氧化锆骨支架有良好的抗冲击性能。上述测试结果如图7所示。此外，与现有研究中陶瓷材料、金属材料和高分子聚合物材料制备的交叉结构、堆叠结构、蜂窝结构等多孔骨支架相比，在压缩载荷下，氧化锆TPMS具有高达46.78kN·mm/g的比强度和4.37J/g的比吸能，在1m/s的冲击载荷下TPMS-C体现出更高的比强度和比吸能。
表1准静态压缩试验与抗冲击试验结果
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。
Claims (5)
1.一种抗冲击可促成骨分化极小曲面骨支架，其特征在于：该极小曲面骨支架由ZrO2、Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒混合在特殊的液体中制成的打印材料经纳米粒子喷射3D打印技术打印所得。
2.如权利要求1所述的一种抗冲击可促成骨分化极小曲面骨支架，其特征在于：按质量百分比计，所述ZrO2、Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒的用量分别为4.64％(wt％)、1.47％(wt％)、0.739％(wt％)、0.47％(wt％)和0.38％(wt％)。
3.如权利要求1所述的一种抗冲击可促成骨分化极小曲面骨支架，其特征在于：ZrO2颗粒粒径为100nm-300nm，Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒粒径为50-150nm。
4.如权利要求1～3任一项所述的一种抗冲击可促成骨分化极小曲面骨支架的制备方法，其特征在于：包括如下步骤：
S1、根据最有利于骨细胞生长原则，3D建模出常规结构Normal-A以及极小曲面骨支架TPMS-B和极小曲面骨支架TPMS-C；
S2、将ZrO2和Y2O3、HfO2、Nb2O5、Cao和Al2O3颗粒按比例混合在特殊的液体中，制成打印材料；
S2、经Carmel1400打印设备将打印材料准确喷射在打印机托盘相应位置以得到半成品；随后，使用30℃的恒温水槽对半成品进行清洗，然后使用100℃的恒温干燥箱对半成品烘干处理2h，最后利用马弗炉在1200～1500℃下进行无压脱脂烧结，得到精密氧化锆TPMS骨支架成品。
5.如权利要求4所述的一种抗冲击可促成骨分化极小曲面骨支架的制备方法，其特征在于：所述步骤S1中，Normal-A的孔直径恒定为750μm；TPMS-B的孔径范围设计为200μm～800μm；TPMS-C孔径范围设计为125μm～800μm。
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