CN117401967A - 一种医用可回弹硅酸钙多孔陶瓷支架的制备方法 - Google Patents
一种医用可回弹硅酸钙多孔陶瓷支架的制备方法 Download PDFInfo
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Abstract
本发明公布了一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，先合成硅酸钙纳米纤维，然后在0℃以下，将硅酸钙纳米纤维与冰粉混匀、压实成型、冰点保温重结晶、冻干、烧结，得到由一维硅酸钙纳米纤维架构的多孔陶瓷支架，本发明公布的硅酸钙多孔陶瓷支架，克服了陶瓷材料的脆性，具备刚性和可回弹性，另外使用冰粉为造孔剂，洁净无污染，且孔径可由冰粉粒径调节，多孔陶瓷支架孔道联通性可由冰粉在冰点的保温重结晶调节。多孔陶瓷表现出高刚度和可回弹性，在生物医学领域有较大应用前景。
Description
技术领域
本发明属于新材料领域，具体涉及一种医用可回弹硅酸钙多孔陶瓷支架的制备方法
背景技术
多孔陶瓷支架是一种在骨科手术中广泛应用的特殊类型的支架或骨植入物。这些支架以其独特的材料特性和结构而著称，通常由陶瓷材料如氧化铝或氧化锆制成，具有高度多孔的结构。这种多孔性不仅有助于支持骨细胞的生长，还可以促进新骨组织的形成，从而加速骨折愈合或骨植入物融合的过程。与传统的金属支架相比，多孔陶瓷支架具有生物相容性更好、不引发金属过敏反应、更接近自然骨的机械性能等优点。然而，它们也存在一些缺点，如脆弱性较高和制造成本较高。因此，在使用多孔陶瓷支架之前，医生通常会根据患者的具体情况仔细评估其可行性和适用性，以确保手术的成功和患者的安全。
硅酸钙多孔陶瓷因为其生物安全性，通常用于骨科和牙科领域，作为骨修复和组织工程的支架。现有技术制备硅酸钙多孔陶瓷，是将含钙化合物，常见的如氧化钙、氢氧化钙等与二氧化硅粉末，添加造孔剂模压成型后高温烧结得到。现有技术制备得到的硅酸钙多孔陶瓷，晶粒形状为颗粒型，孔隙连通性差，高孔隙率时候，力学性能差。申请号为CN202111617687X的中国专利公布了一种多孔硅酸钙陶瓷及其超快速制备方法。该申请使用脱铝后的高铝粉煤灰为硅源制备硅酸钙多孔陶瓷，孔隙结构为颗粒堆积型孔隙结构。
申请号为CN2021104533217的中国专利公布了锰掺杂硅酸钙多孔陶瓷支架及其制备方法和应用，通过3D打印的方法制备硅酸钙多孔陶瓷材料。
申请号为CN2013104397152的中国专利公布了一种利用造孔剂模压的方法制备含锶可降解硅酸钙多孔陶瓷。
申请号为CN2019101171749的中国专利公布了一种孔形可调的硅酸钙多孔陶瓷膜的制备方法，使用溶胶凝胶的方法，制备硅酸钙多孔陶瓷。
现有技术制备的硅酸钙多孔陶瓷支架，存在有机造孔剂残留，易掉粉的问题，容易引发感染，且陶瓷脆性较大，多次吸收脱水后，在表面张力作用下容易开裂损坏的问题。
发明内容
本发明的目的是提供一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，以解决上述背景技术中提出的问题，本发明的技术方案：
将45wt％～62wt％氢氧化钙和38wt％～55wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度为50～500转/分钟，温度为180℃～300℃，反应2～12小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉，20wt％～70wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与30wt％～80wt％的冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温1～12h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1100℃～1400℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为70％～90％，抗压强度为15～30Mpa,具备纤维状孔隙结构，回弹性达到50％。有益效果：本发明公布的硅酸钙多孔陶瓷支架，克服了陶瓷材料的脆性，具备刚性和可回弹性，另外使用冰粉为造孔剂，洁净无污染，且孔径可由冰粉粒径调节，多孔陶瓷支架孔道联通性可由冰粉在冰点的保温重结晶调节。多孔陶瓷表现出高刚度和可回弹性，在生物医学领域有较大应用前景。
附图说明
图1为实施例1制备得到的硅酸钙多孔陶瓷支架的sem图。
图2为实施例1的可回弹压力测试
具体实施方式
下面将结合本发明实施例中的附图，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，仍然属于本发明保护的范围。
实施例1：
一种可回弹硅酸钙多孔陶瓷支架的制备方法，将62wt％氢氧化钙和38wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度500转/分钟，温度为300℃，反应2小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉，70wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与30wt％的粒径为500纳米冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温1h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1400℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为70％，抗压强度为30Mpa,具备纤维状孔隙结构，回弹性达到50％。
实施例2：
一种可回弹硅酸钙多孔陶瓷支架的制备方法，将45wt％氢氧化钙和55wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度50转/分钟，温度为180℃，反应12小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉，50wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与50wt％的粒径为2微米冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温12h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1100℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为80％，抗压强度为24Mpa,具备纤维状孔隙结构，回弹性达到52％。
实施例3：
一种可回弹硅酸钙多孔陶瓷支架的制备方法，将55wt％氢氧化钙和45wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度200转/分钟，温度为200℃，反应4小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉40wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与60wt％的粒径为5微米冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温8h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1300℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为88％，抗压强度为21Mpa,具备纤维状孔隙结构，回弹性达到56％。
实施例4：
一种可回弹硅酸钙多孔陶瓷支架的制备方法，将58wt％氢氧化钙和42wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度100转/分钟，温度为230℃，反应5小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉40wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与60wt％的粒径为10微米冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温8h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1300℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为88％，抗压强度为17Mpa,具备纤维状孔隙结构，回弹性达到60％。
实施例5：
一种可回弹硅酸钙多孔陶瓷支架的制备方法，将53wt％氢氧化钙和47wt％二氧化硅加水混匀，其中液固比为20:1,将混匀后的样品置于带搅拌功能的水热反应釜中，设定搅拌速度100转/分钟，温度为250℃，反应5小时得到均匀浆料，将浆料烘干后得到蓬松硅酸钙纳米纤维粉20wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与80wt％的粒径为10微米冰粉混匀，然后置于低温模具中压实成型，将上述压实成型的样品至于冰点保温6h使冰粉重结晶，将进过重结晶处理的样品冻干，将冻干后的样品1200℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。制备得到的可回弹硅酸钙多孔陶瓷支架孔隙率为98％，抗压强度为15Mpa,具备纤维状孔隙结构，回弹性达到70％。
Claims (6)
1.一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，其特征包括下述步骤：步骤1，将45wt％～62wt％氢氧化钙和38wt％～55wt％二氧化硅原料水热反应制备硅酸钙纳米纤维；步骤2，将20wt％～70wt％上述硅酸钙纳米纤维在0℃下预先冷冻后与30wt％～80wt％的冰粉混匀，然后置于零度以下低温模具中压实成型；步骤3，将上述压实成型的样品置于冰点保温1～12h使冰粉重结晶；步骤4，将经过重结晶处理的样品冻干；步骤5，将冻干后的样品1100℃～1400℃热处理得到医用可回弹硅酸钙多孔陶瓷支架。
2.根据权利要求1，一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，所述水热反应的搅拌速度为50～500转/分钟。
3.根据权利要求1，一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，所述水热反应釜的温度为180℃～300℃。
4.根据权利要求1，一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，所制备得到的医用硅酸钙多孔陶瓷支架的的孔隙率为70％～90％。
5.根据权利要求1，一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，所制备得到的医用硅酸钙多孔陶瓷支架的抗压强度为15～30Mpa。
6.根据权利要求1，一种医用可回弹硅酸钙多孔陶瓷支架的制备方法，所制备得到的医用硅酸钙多孔陶瓷支架弹性变形达到50％。
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