CN104803671B - 一种磷酸三钙/氧化锆生物陶瓷及其制备方法 - Google Patents

一种磷酸三钙/氧化锆生物陶瓷及其制备方法 Download PDF

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CN104803671B
CN104803671B CN201510146812.1A CN201510146812A CN104803671B CN 104803671 B CN104803671 B CN 104803671B CN 201510146812 A CN201510146812 A CN 201510146812A CN 104803671 B CN104803671 B CN 104803671B
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zirconium oxide
tricalcium phosphate
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CN104803671A (zh
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朱礼飞
张劲松
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Jiangsu Hanren Biotechnology Co ltd
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Abstract

本发明公开了一种磷酸三钙/氧化锆生物陶瓷及其制备方法，涉及生物材料领域，由以下质量份数的各个组分制备而成：磷酸三钙40‑60份、氧化锆20‑40份、硅酸钙5‑15份、纳米氧化钛3‑6份、麦饭石粉3‑6份、偏磷酸钾4‑9份和纳米氧化钨2‑5份。一种磷酸三钙/氧化锆生物陶瓷的制备方法，制备步骤如下：（1）称量；（2）球磨；（3）冷压成型；（4）高温煅烧；（5）冷却。本发明提供的磷酸三钙/氧化锆生物陶瓷生物相容性较好，生物活性较高，同时具有良好的抗压强度和断裂韧性，是一种理想的骨骼修复替代材料。

Description

一种磷酸三钙/氧化锆生物陶瓷及其制备方法
技术领域
本发明属于生物材料领域，特别涉及一种磷酸三钙/氧化锆生物陶瓷及该生物陶瓷的制备方法。
背景技术
随着材料科技的发展，生物材料因其对机体组织进行修复、替代与再生的特殊性能，已经成为当今生物医学领域重要的研究方向之一。生物硬组织代用材料最早是使用体骨、动物骨，后来发展到采用不锈钢和塑料，由于不锈钢存在溶析、腐蚀和疲劳问题，塑料存在稳定性差和强度低的问题。因此造成生物材料发展的瓶颈，生物陶瓷的出现，改善了现有替代材料的不足，因其诸多优势，因此，生物陶瓷具有了广阔的发展前景。
磷酸钙陶瓷(CPC)是生物活性陶瓷材料中的重要种类，目前研究和应用最多的是羟基磷灰石(HA)和磷酸三钙(TCP)。磷酸钙陶瓷含有CaO和P2O5两种成份，是构成人体硬组织的重要无机物质，植入人体后，其表面同人体组织可通过键的结合，达到完全亲和。
其中，磷酸三钙(TCP)中，目前广泛应用的生物降解陶瓷β-磷酸三钙(简称β-TCP)，属三方晶系，钙磷原子比为1.5，是磷酸钙的一种高温相。β-TCP的最大优势就是生物相容性好，植入机体后与骨直接融合，无任何局部炎性反应及全身毒副作用。
钙磷比在决定体内溶解性和吸收趋势上起着重要作用，所以和HA相比TCP更易于在体内溶解，其溶解度约比HA高10-20倍。常用的β-TCP植入体内可逐渐降解，降解速率可因其表面构造，结晶构型，含孔率及植入动物的不同而异，其强度常随降解而减弱。
与其他陶瓷相比，β-TCP陶瓷更类似于人骨和天然牙的性质和结构在生物体内，羟基磷灰石的溶解是无害的，并且依靠从体液中补充钙和磷酸根离子等形成新骨，可在骨骼接合界面产生分解、吸收和析出等反应，实现牢固结合。
β-TCP陶瓷的缺点是机械强度偏低，经不起力的冲击。将β-TCP与其他材料混合，制成双相或多相陶瓷，是提高其力学强度的方法之一。
发明内容
本发明解决的技术问题：针对上述不足，克服现有技术的缺陷，本发明的目的是提供一种磷酸三钙/氧化锆生物陶瓷及其制备方法。
本发明的技术方案：一种磷酸三钙/氧化锆生物陶瓷，由以下质量份数的各个组分制备而成：
磷酸三钙40-60份、氧化锆20-40份、硅酸钙5-15份、纳米氧化钛3-6份、麦饭石粉3-6份、偏磷酸钾4-9份和纳米氧化钨2-5份。
作为优选，各个组分的质量份数为：磷酸三钙45-58份、氧化锆25-36份、硅酸钙9-12份、纳米氧化钛4-5份、麦饭石粉4-5份、偏磷酸钾6-8份和纳米氧化钨3-4份。
作为优选，各个组分的质量份数为：磷酸三钙52份、氧化锆32份、硅酸钙10份、纳米氧化钛4份、麦饭石粉5份、偏磷酸钾7份和纳米氧化钨3份。
一种磷酸三钙/氧化锆生物陶瓷的制备方法，制备步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体进行冷压成型；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1100℃-1350℃，压力300-700MPa，时间2-8h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
作为优选，步骤（4）中煅烧的温度为1200℃。
作为优选，步骤（4）中煅烧的压力为580MPa。
有益效果：本发明提供的磷酸三钙/氧化锆生物陶瓷，是一种复合生物活性陶瓷，磷酸三钙生物活性陶瓷具有十分理想的生物相容性，且可缓慢释放钙磷离子，但是其力学性能较不理想；氧化锆生物陶瓷是生物惰性陶瓷，生物相容性较好，力学性能较好，但是并不具备生物活性，因此，两两种生物陶瓷材料结合在一起，制备双相复合生物陶瓷，不仅继承了磷酸三钙优良的生物活性，且提高了生物陶瓷的力学性能。
因此，本发明提供的磷酸三钙/氧化锆生物陶瓷生物相容性较好，生物活性较高，同时具有良好的抗压强度和断裂韧性，是一种理想的骨骼修复替代材料。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明优选实施方案进行描述，但是应当理解， 这些描述只是为进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
实施例 1：
一种磷酸三钙/氧化锆生物陶瓷，包括以下质量份数的各个组分：
磷酸三钙40份、氧化锆20份、硅酸钙5份、纳米氧化钛3份、麦饭石粉3份、偏磷酸钾4份和纳米氧化钨2份。
根据本发明提供的制备方法制备磷酸三钙/氧化锆生物陶瓷，步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体采用60T压机进行压制；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1300℃，压力400MPa，时间4h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
对得到的块状磷酸三钙/氧化锆生物陶瓷进行检测，检测生物陶瓷的性能：硬度1020HV；压缩强度1790MPa；抗弯强度780MPa；韧性16MPa·m1/2。
实施例 2：
一种磷酸三钙/氧化锆生物陶瓷，包括以下质量份数的各个组分：
磷酸三钙60份、氧化锆40份、硅酸钙15份、纳米氧化钛6份、麦饭石粉6份、偏磷酸钾9份和纳米氧化钨5份。
根据本发明提供的制备方法制备磷酸三钙/氧化锆生物陶瓷，步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体采用60T压机进行压制；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1300℃，压力400MPa，时间7h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
对得到的块状磷酸三钙/氧化锆生物陶瓷进行检测，检测生物陶瓷的性能：硬度1050HV；压缩强度1820MPa；抗弯强度830MPa；韧性18MPa·m1/2。
实施例 3：
一种磷酸三钙/氧化锆生物陶瓷，包括以下质量份数的各个组分：
磷酸三钙45份、氧化锆25份、硅酸钙9份、纳米氧化钛4份、麦饭石粉4份、偏磷酸钾6份和纳米氧化钨3份。
根据本发明提供的制备方法制备磷酸三钙/氧化锆生物陶瓷，步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体采用60T压机进行压制；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1200℃，压力580MPa，时间6h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
对得到的块状磷酸三钙/氧化锆生物陶瓷进行检测，检测生物陶瓷的性能：硬度1030HV；压缩强度1810MPa；抗弯强度790MPa；韧性16MPa·m1/2。
实施例4：
一种磷酸三钙/氧化锆生物陶瓷，包括以下质量份数的各个组分：
磷酸三钙58份、氧化锆36份、硅酸钙12份、纳米氧化钛5份、麦饭石粉5份、偏磷酸钾8份和纳米氧化钨4份。
根据本发明提供的制备方法制备磷酸三钙/氧化锆生物陶瓷，步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体采用60T压机进行压制；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1200℃，压力580MPa，时间6h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
对得到的块状磷酸三钙/氧化锆生物陶瓷进行检测，检测生物陶瓷的性能：硬度1040HV；压缩强度1810MPa；抗弯强度800MPa；韧性17MPa·m1/2。
实施例5：
一种磷酸三钙/氧化锆生物陶瓷，包括以下质量份数的各个组分：
磷酸三钙52份、氧化锆32份、硅酸钙10份、纳米氧化钛4份、麦饭石粉5份、偏磷酸钾7份和纳米氧化钨3份。
根据本发明提供的制备方法制备磷酸三钙/氧化锆生物陶瓷，步骤如下：
（1）称量：准确称取各个组分；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体采用60T压机进行压制；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1200℃，压力580MPa，时间5h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
对得到的块状磷酸三钙/氧化锆生物陶瓷进行检测，检测生物陶瓷的性能：硬度1040HV；压缩强度1820MPa；抗弯强度800MPa；韧性17MPa·m1/2。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (5)

1.一种磷酸三钙/氧化锆生物陶瓷的制备方法，其特征在于，制备步骤如下：
（1）称量：准确称取各个组分，磷酸三钙40-60份、氧化锆20-40份、硅酸钙5-15份、纳米氧化钛3-6份、麦饭石粉3-6份、偏磷酸钾4-9份和纳米氧化钨2-5份；
（2）球磨：将各个组分混合在一起，放入球磨机进行研磨混合；
（3）冷压成型：将混合粉体进行冷压成型；
（4）粉体成型后放入模具中，进行高温煅烧，温度为1100℃-1350℃，压力300-700MPa，时间2-8h；
（5）煅烧之后，待冷却取出，即得到块状磷酸三钙/氧化锆生物陶瓷。
2.根据权利要求1所述的磷酸三钙/氧化锆生物陶瓷的制备方法，其特征在于：步骤（4）中煅烧的温度为1200℃。
3.根据权利要求1所述的磷酸三钙/氧化锆生物陶瓷的制备方法，其特征在于：步骤（4）中煅烧的压力为580MPa。
4.根据权利要求1所述的磷酸三钙/氧化锆生物陶瓷的制备方法，其特征在于：步骤（1）中各个组分的质量份数为：磷酸三钙45-58份、氧化锆25-36份、硅酸钙9-12份、纳米氧化钛4-5份、麦饭石粉4-5份、偏磷酸钾6-8份和纳米氧化钨3-4份。
5.根据权利要求4所述的磷酸三钙/氧化锆生物陶瓷的制备方法，其特征在于：步骤（1）中各个组分的质量份数为：磷酸三钙52份、氧化锆32份、硅酸钙10份、纳米氧化钛4份、麦饭石粉5份、偏磷酸钾7份和纳米氧化钨3份。
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