CN106830899A - 一种复合陶瓷材料及其制备方法与应用 - Google Patents

一种复合陶瓷材料及其制备方法与应用 Download PDF

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CN106830899A
CN106830899A CN201611244913.3A CN201611244913A CN106830899A CN 106830899 A CN106830899 A CN 106830899A CN 201611244913 A CN201611244913 A CN 201611244913A CN 106830899 A CN106830899 A CN 106830899A
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composite ceramic
zirconium oxide
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CN106830899B (zh
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曹蓓蓓
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Hagong Ningbo medical technology Taizhou Co.,Ltd.
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Guangzhou Kai Yao Asset Management Co Ltd
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Abstract

本发明属于陶瓷材料制备领域，具体涉及一种复合陶瓷材料及其制备方法与应用。本发明以聚乙烯吡咯烷酮和三嵌段聚醚P123作为模板剂，将其与锆酸丁酯、氯化铝形成骨架的前驱体混合，前驱体在酸性条件下水解并沉积在模板剂聚集体的周围，从而形成一种有序的介观结构，通过煅烧除去模板剂，得到具有介孔结构的纳米氧化铝‑氧化锆复合材料；然后在pH为8～11的条件下，采用氢氧化钙和磷酸作为反应物，在纳米氧化铝‑氧化锆复合材料表面形成纳米羟基磷灰石晶核，得到表面包覆羟基磷灰石的纳米氧化铝‑氧化锆复合材料，该复合材料进一步冷压成型、烧结，得到复合陶瓷材料。本发明制得的复合陶瓷材料是一种非常理想的骨骼替代修复材料。

Description

一种复合陶瓷材料及其制备方法与应用
技术领域
本发明属于陶瓷材料制备领域，具体涉及一种复合陶瓷材料及其制备方法与应用。
背景技术
生物陶瓷是指用作特定的生物或生理功能的一类陶瓷材料，即直接用于人体或与人体直接相关的生物、医用、生物化学等的陶瓷材料。作为生物陶瓷材料，需具备如下条件：生物相容性、力学相容性、与生物组织有优异的亲和性、抗血栓、灭菌性并具有很好的物理、化学稳定性。生物陶瓷材料分为生物惰性陶瓷材料和生物活性陶瓷材料。
生物惰性陶瓷主要是指化学性能稳定、生物相溶性好的陶瓷材料。如氧化铝、氧化锆以及医用碳素材料等。这类陶瓷材料的结构都比较稳定，分子中的键合力较强，而且都具有较高的强度、耐磨性及化学稳定性。氧化铝陶瓷是应用最为广泛的生物惰性陶瓷之一。氧化铝陶瓷植入人体后表面生成极薄的纤维膜，界面无化学反应，多用于全臀复位修复术及股骨和髋骨部连接。但其弯曲强度和韧性较低，在使用过程中容易产生脆性断裂。此外高纯超细α-Al2O3粉体加工成型困难，不易烧结。上述因素制约着氧化铝生物陶瓷材料在人工髋关节领域的应用，因此在保证氧化铝纯度的前提下，能否有效促进氧化铝材料烧结、提高氧化铝陶瓷的断裂韧性和弯曲强度决定该材料能否成功并大规模应用的关键。
生物活性陶瓷包括表面生物活性陶瓷和生物吸收性陶瓷，又叫生物降解陶瓷。生物表面活性陶瓷通常含有羟基，还可做成多孔性，生物组织可长入并同其表面发生牢固的键合；生物吸收性陶瓷的特点是能部分吸收或者全部吸收，在生物体内能诱发新生骨的生长。生物活性陶瓷具有骨传导性，它作为一个支架，成骨在其表面进行；它还可作为多种物质的外壳或填充骨缺损。生物活性陶瓷有生物活性玻璃、羟基磷灰石陶瓷、磷酸三钙陶瓷等几种。
羟基磷灰石(hydroxyapatite，简称HA或HAP)组成与天然磷灰石矿物相近，是脊椎动物骨和齿的主要无机成分，结构亦非常接近，呈片状微晶状态。它作为骨代替物被用于骨移植。HA有良好的生物相容性，植入体内不仅安全，无毒，还能传导骨生长。HA能使骨细胞附着在其表面，随着新骨的生长，这个连接地带逐渐萎缩，并且HA通过晶体外层成为骨的一部分，新骨可以从HA植入体与原骨结合处沿着植入体表面或内部贯通性孔隙攀附生长。但是HA机械强度较差，不耐磨，只限用于不承受大载荷部位。
如果将两种生物惰性陶瓷材料和生物活性陶瓷材料结合在一起，做到优势互补，得到的复合生物陶瓷将具备较好的使用前景。
发明内容
为了克服现有技术的不足与缺点，本发明的首要目的在于提供一种复合陶瓷材料的制备方法。
本发明的另一目的在于提供上述制备方法制备得到的复合陶瓷材料。
本发明的再一目的在于提供上述复合陶瓷材料的应用。
本发明的目的通过下述技术方案实现：
一种复合陶瓷材料的制备方法，包含如下步骤：
(1)将锆酸丁酯和氯化铝加入到浓盐酸中，搅拌均匀，得到透明澄清的复合前驱体溶液；将模板剂聚乙烯吡咯烷酮和模板剂三嵌段聚醚P123溶于无水乙醇，得到复合模板剂溶液；
(2)将步骤(1)制得的复合前驱体溶液与复合模板剂溶液混合均匀，20～40℃静置反应20～30h，然后将反应产物干燥，400℃～500℃煅烧5h～7h，冷却，得到具有介孔结构的纳米氧化铝-氧化锆复合材料；
(3)将步骤(2)制得的纳米氧化铝-氧化锆复合材料均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；
(4)搅拌条件下，将磷酸溶液滴加到步骤(3)制得的混合物中，滴加完成后，在pH为8～11的条件下，继续搅拌反应1～2h；然后将反应产物干燥，600～700℃煅烧4～5h，冷却，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料；
(5)将步骤(4)制得的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进行冷压成型；然后在温度为1000～1400℃，压力为1.5～2.5GPa，时间为0.5～1h的条件下进行烧结；冷却，得到复合陶瓷材料；
步骤(1)中所述的锆酸丁酯和氯化铝质量比优选为1:(0.5～1)；
步骤(1)中所述的浓盐酸的质量分数优选为36％～38％；
步骤(1)中所述的聚乙烯吡咯烷酮和三嵌段聚醚P123的质量比优选为(3～5):1；
步骤(1)中所述的锆酸丁酯和氯化铝与模板剂(聚乙烯吡咯烷酮和三嵌段聚醚P123)的物质的量之比为1:(0.001～0.01)；
步骤(1)中所述的浓盐酸和无水乙醇的体积比为(1～5):20；
步骤(2)中所述的静置反应的条件优选为30℃静置反应24h；
步骤(2)中所述的干燥优选为自然干燥；
步骤(2)中所述的煅烧的条件优选为450℃煅烧6h；
步骤(3)中所述的混合物中纳米氧化铝-氧化锆复合材料的质量分数为10～15％；
步骤(4)中所述的搅拌的转速优选为50～100r/min；
步骤(4)中所述的磷酸溶液的浓度优选为0.3mol/L；
步骤(4)中滴加完成后反应体系中Ca/P摩尔比优选为1.67:1；
步骤(4)中所述的继续搅拌反应的条件优选为：在pH为10的条件下继续搅拌反应1.5h；
步骤(4)中所述的干燥优选为自然干燥；
步骤(4)中所述的煅烧的条件优选为650℃煅烧4.5h；
步骤(4)中所述的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料中羟基磷灰石与纳米氧化铝-氧化锆复合材料的质量比优选为1:(1～5)。
一种复合陶瓷材料，通过上述制备方法制备得到。
所述的复合陶瓷材料在人造骨、人工关节及人造齿根制备领域中的应用。
本发明的原理：
本发明将聚乙烯吡咯烷酮和三嵌段聚醚P123作为模板剂，与锆酸丁酯、氯化铝形成骨架的前驱体混合，前驱体在酸性条件下水解并沉积在模板剂聚集体的周围，从而形成一种有序的介观结构，通过煅烧除去模板剂，得到具有介孔结构的纳米氧化铝-氧化锆复合材料。然后在pH为8～11的条件下，采用氢氧化钙和磷酸作为反应物，在短时间内，在纳米氧化铝-氧化锆复合材料表面形成纳米羟基磷灰石晶核，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料，其中，反应时间以及反应pH决定了晶粒来不及迅速长大，为得到细小晶粒提供了保证。将得到的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进一步冷压成型、烧结，得到复合陶瓷材料。
本发明相对于现有技术具有如下的优点及效果：
(1)本发明采用聚乙烯吡咯烷酮和三嵌段聚醚P123作为模板剂，制得的复合陶瓷材料连通性比较好，孔径大小和孔的分布都很均匀，介孔结构有利于其在体内的降解，也有利于骨细胞和营养物质的运输，从而促进新骨的生长。
(2)本发明将氧化铝、氧化锆和羟基磷灰石三者进行结合，制得的复合陶瓷材料克服了氧化铝陶瓷弯曲强度和韧性较低，在使用过程中容易产生脆性断裂以及HA机械强度较差，不耐磨等缺点，延续了氧化铝和羟基磷灰石优良的作用，进一步提高了生物陶瓷的力学性能和韧性，是一种非常理想的骨骼替代修复材料。
(3)本发明没有使用制孔剂，烧结过程不会留下危害生物活性的残余物质，也不会产生有副作用的降解产物。
(4)本发明采用沉淀法在纳米氧化铝-氧化锆复合材料表面生成纳米羟基磷灰石晶核，纳米羟基磷灰石晶核与纳米氧化铝-氧化锆复合材料结合紧密，不仅没有影响其生物相容性，反而更好地提高了生物陶瓷的力学性能。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例中所述的浓盐酸质量分数为37％；
实施例1
(1)将锆酸丁酯和氯化铝按照质量比1:0.8加入到浓盐酸中，搅拌均匀，得到透明澄清的复合前驱体溶液；将模板剂聚乙烯吡咯烷酮和模板剂三嵌段聚醚P123按照质量比4:1溶于无水乙醇，得到复合模板剂溶液；其中，锆酸丁酯和氯化铝与模板剂(聚乙烯吡咯烷酮和三嵌段聚醚P123)的物质的量之比为1:0.006；浓盐酸和无水乙醇的体积比为3:20；
(2)将步骤(1)制得的复合前驱体溶液与复合模板剂溶液混合均匀，30℃静置反应24h，将反应产物自然干燥，450℃煅烧6h，自然冷却，得到具有介孔结构的纳米氧化铝-氧化锆复合材料；
(3)将步骤(2)制得的纳米氧化铝-氧化锆复合材料粉体均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；其中，混合物中纳米氧化铝-氧化锆复合材料的质量分数为12％；
(4)在搅拌(转速为60r/min)条件下，将0.3mol/L的磷酸溶液滴加到步骤(3)制得的混合物中，滴加完成后，反应体系中Ca/P摩尔比为1.67:1；然后在pH为10的条件下，继续搅拌反应1.5h；将反应产物自然干燥，650℃煅烧4.5h，自然冷却，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料；其中，表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料中羟基磷灰石与纳米氧化铝-氧化锆复合材料的质量比为1:2；
(5)将步骤(4)制得的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进行冷压成型；然后在温度为1200℃，压力为2.0GPa，时间为0.6h的条件下进行烧结；冷却，得到复合陶瓷材料。
实施例2
(1)将锆酸丁酯和氯化铝按照质量比1:0.5加入到浓盐酸中，搅拌均匀，得到透明澄清的复合前驱体溶液；将模板剂聚乙烯吡咯烷酮和模板剂三嵌段聚醚P123按照质量比3:1溶于无水乙醇，得到复合模板剂溶液；其中，锆酸丁酯和氯化铝与模板剂(聚乙烯吡咯烷酮和三嵌段聚醚P123)的物质的量之比为1:0.001；浓盐酸和无水乙醇的体积比为1:20；
(2)将步骤(1)制得的复合前驱体溶液与复合模板剂溶液混合均匀，20℃静置反应30h，将反应产物自然干燥，400℃煅烧7h，自然冷却，得到具有介孔结构的纳米氧化铝-氧化锆复合材料；
(3)将步骤(2)制得的纳米氧化铝-氧化锆复合材料粉体均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；其中，混合物中纳米氧化铝-氧化锆复合材料的质量分数为15％；
(4)在搅拌(转速为100r/min)条件下，将0.3mol/L的磷酸溶液滴加到步骤(3)制得的混合物中，滴加完成后，反应体系中Ca/P摩尔比为1.67:1；然后在pH为8的条件下，继续搅拌反应2h；将反应产物自然干燥，700℃煅烧4h，自然冷却，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料；其中，表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料中羟基磷灰石与纳米氧化铝-氧化锆复合材料的质量比为1:1；
(5)将步骤(4)制得的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进行冷压成型；然后在温度为1000℃，压力为2.5GPa，时间为1h的条件下进行烧结；冷却，得到复合陶瓷材料。
实施例3
(1)将锆酸丁酯和氯化铝按照质量比1:1加入到浓盐酸中，搅拌均匀，得到透明澄清的复合前驱体溶液；将模板剂聚乙烯吡咯烷酮和模板剂三嵌段聚醚P123按照质量比5:1溶于无水乙醇，得到复合模板剂溶液；其中，锆酸丁酯和氯化铝与模板剂(聚乙烯吡咯烷酮和三嵌段聚醚P123)的物质的量之比为1:0.01；浓盐酸和无水乙醇的体积比为5:20；
(2)将步骤(1)制得的复合前驱体溶液与复合模板剂溶液混合均匀，40℃静置反应20h，将反应产物自然干燥，500℃煅烧5h，自然冷却，得到具有介孔结构的纳米氧化铝-氧化锆复合材料；
(3)将步骤(2)制得的纳米氧化铝-氧化锆复合材料粉体均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；其中，混合物中纳米氧化铝-氧化锆复合材料的质量分数为10％；
(4)在搅拌(转速为50r/min)条件下，将0.3mol/L的磷酸溶液滴加到步骤(3)制得的混合物中，滴加完成后，反应体系中Ca/P摩尔比为1.67:1；然后在pH为11的条件下，继续搅拌反应1h；将反应产物自然干燥，600℃煅烧5h，自然冷却，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料；其中，表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料中羟基磷灰石与纳米氧化铝-氧化锆复合材料的质量比为1:5；
(5)将步骤(4)制得的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进行冷压成型；然后在温度为1400℃，压力为1.5GPa，时间为0.5h的条件下进行烧结；冷却，得到复合陶瓷材料。
对比实施例
(1)将纳米氧化铝粉体均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；其中，混合物中纳米氧化铝的质量分数为12％；
(2)在搅拌(转速为60r/min)条件下，将0.3mol/L的磷酸溶液滴加到步骤(1)制得的混合物中，滴加完成后，反应体系中Ca/P摩尔比为1.67:1；然后在pH为10的条件下，继续搅拌反应1.5h；将反应产物自然干燥，650℃煅烧4.5h，自然冷却，得到表面包覆羟基磷灰石的纳米氧化铝材料；其中，表面包覆羟基磷灰石的纳米氧化铝材料中羟基磷灰石与纳米氧化铝的质量比为1:2；
(3)将步骤(2)制得的表面包覆羟基磷灰石的纳米氧化铝材料进行冷压成型；然后在温度为1200℃，压力为2.0GPa，时间为0.6h的条件下进行烧结；冷却，得到复合陶瓷材料。
效果实施例
对实施例1～3以及对比实施例制得的复合陶瓷材料进行性能测试，结果如表1：
表1复合陶瓷材料的性能测试结果
硬度 压缩强度 抗弯强度 韧性
实施例1 1070HV 1830MPa 620MPa
实施例2 985HV 1750MPa 600MPa
实施例3 960HV 1690MPa 585MPa
对比实施例 750HV 1200MPa 470MPa
与对比实施例相比，本发明实施例1～3制得的复合陶瓷材料具有更好的硬度、压缩强度、抗弯强度和韧性，说明将氧化铝、氧化锆和羟基磷灰石三者进行科学结合，制得的复合陶瓷材料克服了氧化铝陶瓷弯曲强度和韧性较低，在使用过程中容易产生脆性断裂以及HA机械强度较差，不耐磨等缺点，延续了氧化铝和羟基磷灰石优良的作用，进一步提高了生物陶瓷的力学性能和韧性，是一种非常理想的骨骼替代修复材料。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种复合陶瓷材料的制备方法，其特征在于，所述方法包含如下步骤：
(1)将锆酸丁酯和氯化铝加入到浓盐酸中，搅拌均匀，得到透明澄清的复合前驱体溶液；将模板剂聚乙烯吡咯烷酮和模板剂三嵌段聚醚P123溶于无水乙醇，得到复合模板剂溶液；
(2)将步骤(1)制得的复合前驱体溶液与复合模板剂溶液混合均匀，20～40℃静置反应20～30h，然后将反应产物干燥，400℃～500℃煅烧5h～7h，冷却，得到具有介孔结构的纳米氧化铝-氧化锆复合材料；
(3)将步骤(2)制得的纳米氧化铝-氧化锆复合材料均匀分散于乙二醇中，然后加入氢氧化钙，混合均匀，得到混合物；
(4)搅拌条件下，将磷酸溶液滴加到步骤(3)制得的混合物中，滴加完成后，在pH为8～11的条件下，继续搅拌反应1～2h；然后将反应产物干燥，600～700℃煅烧4～5h，冷却，得到表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料；
(5)将步骤(4)制得的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料进行冷压成型；然后在温度为1000～1400℃，压力为1.5～2.5GPa，时间为0.5～1h的条件下进行烧结；冷却，得到复合陶瓷材料。
2.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(1)中所述的锆酸丁酯和氯化铝质量比为1:0.5～1，步骤(1)中所述的浓盐酸的质量分数为36％～38％。
3.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(1)中所述的聚乙烯吡咯烷酮和三嵌段聚醚P123的质量比为3～5:1。
4.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(1)中所述的锆酸丁酯和氯化铝的混合物与模板剂聚乙烯吡咯烷酮和三嵌段聚醚P123的混合物物质的量之比为1:0.001～0.01。
5.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(1)中所述的浓盐酸和无水乙醇的体积比为1～5:20。
6.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(3)中所述的混合物中纳米氧化铝-氧化锆复合材料的质量分数为10％～15％。
7.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(4)中所述的磷酸溶液的浓度为0.3mol/L；步骤(4)中滴加完成后反应体系中Ca/P摩尔比为1.67：1。
8.根据权利要求1所述的复合陶瓷材料的制备方法，其特征在于：
步骤(4)中所述的表面包覆羟基磷灰石的纳米氧化铝-氧化锆复合材料中羟基磷灰石与纳米氧化铝-氧化锆复合材料的质量比为1:1～5。
9.一种复合陶瓷材料，其特征在于通过权利要求1～8任一项所述的制备方法制备得到。
10.一种如权利要求9所述的复合陶瓷材料在人造骨、人工关节及人造齿根制备领域中的应用。
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