CN110078480B - 一种人工关节用陶瓷复合材料及其制备方法 - Google Patents
一种人工关节用陶瓷复合材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011787 zinc oxide Substances 0.000 claims abstract description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000292 calcium oxide Substances 0.000 claims abstract description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 7
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 6
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
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- 238000000034 method Methods 0.000 claims description 11
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- 210000004394 hip joint Anatomy 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
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Abstract
本发明属于生物材料领域，具体涉及一种人工关节用陶瓷复合材料及其制备方法，人工关节用陶瓷复合材料，由以下重量份的各组分组成：氧化铝60‑90份、氧化锆10‑30份、氧化铝纤维3‑8份、氧化锌0‑2份、氧化钙0‑5份、氧化镁0‑5份，所述氧化锆中含有氧化铪杂质，所述氧化铪杂质含量占氧化锆总质量的5%以下。本发明添加的氧化铝纤维具有较高的弹性和压缩强度，有利于增加陶瓷复合材料的韧性，减小陶瓷复合材料发生碎裂的可能；采用KH550对氧化铝纤维进行改性，可以在氧化铝纤维周围包覆较大的集团，从而使纤维之间不能紧密接触，且KH550中的氨基有利于改性后纤维在水中的分散，避免团聚，增加氧化铝纤维在浆料中的分散性，从而增加纤维在陶瓷复合材料中的分散性。
Description
技术领域
本发明属于生物材料领域，具体涉及一种人工关节用陶瓷复合材料及其制备方法。
背景技术
迄今为止，人工关节技术已取得了巨大的成功，人工关节所采用的材料主要有金属、聚合物和陶瓷材料。最早被用作人工关节的是金属材料，其具有非常好的强度、韧性以及加工成型性，但由于其存在应力遮挡，而且因其生物相容性和耐磨耐蚀性较差而容易引起周围组织的慢性炎症等，所以金属材料并不是最适宜的关节材料，随后的超高分子量聚乙烯因在长期使用过程中产生的磨损碎屑引起骨骼发炎、发生无菌性松动和假体脱落等问题而导致需要更换新的人工关节，于是，氧化铝陶瓷因具有高硬度、高弹性模量、高强度、优良的耐磨性以及良好的生物相容性而最早被选择作为制造人工关节的陶瓷材料。
但是，氧化铝陶瓷为硬脆材料，其抗拉强度和断裂韧性很低，氧化铝陶瓷的硬脆特性不仅加工困难，而且有很高的破碎风险。中国专利CN109133885A公开了一种氧化锌掺杂的抗菌人工髋关节陶瓷球头的制备方法，采用氧化锆作为增韧剂增韧氧化铝陶瓷，来增强氧化铝陶瓷材料的断裂韧性和断裂强度，并通过添加氧化锌来提高陶瓷材料的抗菌性能，其所制备的陶瓷材料抗菌率达到65-98％，弯曲强度达到395-514MPa。中国专利CN108689699A公开了一种高柔韧性人工骨骼关节用陶瓷复合材料及制备方法，采用30-40％的羟基磷灰石和30-40％的钇稳定氧化锆增韧氧化铝陶瓷(一方面可以提高氧化铝陶瓷的抗折强度和断裂韧性，另一方面其价格远低于氧化锆陶瓷，具有比氧化锆陶瓷更优的性价比)作为主体材料，并添加5-10％的陶瓷晶须，5-10％的纳米氧化钛，0-10％的牡蛎壳粉，0-10％的氧化镁和0-10％的氧化钙来制备该高柔韧性人工骨骼关节用陶瓷复合材料，其所制备的复合材料虽然断裂韧性高于普通陶瓷材料，但其抗弯强度和压缩强度都低于普通陶瓷材料。
发明内容
为了解决现有陶瓷复合材料无法同时具备高强度和高韧性的问题，本发明公开了一种人工关节用陶瓷复合材料及其制备方法，该陶瓷复合材料通过氧化铝纤维提高陶瓷材料的韧性。
为了实现上述目的，本发明采用如下技术方案:
一种人工关节用陶瓷复合材料，其特征在于：由以下重量份的各组分组成：氧化铝60-90份、氧化锆10-30份、氧化铝纤维3-10份、氧化锌0-2份、氧化钙0-5份、氧化镁0-5份。
作为优选，上述氧化锆中含有氧化铪杂质，所述氧化铪杂质含量占氧化锆总质量的5％以下。添加氧化铝纤维有助于增加陶瓷复合材料的韧性。
作为优选，上述人工关节用陶瓷复合材料由以下重量份的各组分组成：氧化铝70-80份、氧化锆15-25份、氧化铝纤维5-8份、氧化锌0-2份、氧化钙0-5份、氧化镁0-5份。
作为优选，上述氧化锆为氧化钇稳定的氧化锆。
一种人工关节用陶瓷复合材料的制备方法，包括如下步骤：
(1)按比例称取各组分，加入去离子水，搅拌均匀配成浆料，然后在球磨机中对上述浆料进行球磨，得到分散均匀的浆料；
(2)对步骤(1)中分散均匀的浆料进行喷雾干燥，得到造粒料；
(3)将步骤(2)中的造粒料冷压成型；
(4)将步骤(3)中的成型品放入模具中，在真空下或惰性气体保护下进行高温煅烧，煅烧温度为1100-1300℃，时间为1-5h，然后待自然冷却取出即可。
作为优选，上述步骤(1)所用的氧化铝纤维为经硅烷偶联剂KH550改性氧化铝纤维。采用KH550对氧化铝纤维进行改性，可以在氧化铝纤维周围包覆较大的集团，从而使纤维之间不能紧密接触，距离增大，而且KH550中的氨基有利于改性后纤维在水中的分散，增加氧化铝纤维在浆料中的分散性，从而增加纤维在陶瓷复合材料中的分散性。此外，在步骤(4)进行高温煅烧的过程中，纤维改性所引入的偶联剂在高温下发生分解，其中的碳形成活性碳原子，氨基分解产生活性氮原子，碳和氮均深入到陶瓷复合材料中，此过程中会在陶瓷复合材料的表层形成氮化碳、氮化硅(偶联剂中含有Si)、碳化硅等超硬物质，增加陶瓷复合材料的硬度，进一步提高耐磨性。
作为优选，上述步骤(4)中高温煅烧的时间为3-5h。较长的高温煅烧时间有利于充分的进行渗氮和渗碳。
作为优选，上述步骤(1)中去离子水与各组分总量的质量比为2:1-1.5。
作为优选，上述步骤(1)中球磨过程中的料球比为1:0.5-1.5。
本发明具有如下的有益效果：(1)本发明添加的氧化铝纤维具有较高的弹性和压缩强度，有利于增加陶瓷复合材料的韧性，最大限度地减小陶瓷复合材料发生碎裂的可能；
(2)采用硅烷偶联剂KH550对氧化铝纤维进行改性，可以在氧化铝纤维周围包覆较大的集团，从而使纤维之间不能紧密接触，距离增大，而且KH550中的氨基有利于改性后纤维在水中的分散，避免团聚，增加氧化铝纤维在浆料中的分散性，从而增加纤维在陶瓷复合材料中的分散性；
(3)在对成型品进行高温煅烧的过程中，纤维改性所引入的偶联剂在高温下发生分解，其中的碳形成活性碳原子，氨基分解产生活性氮原子，碳和氮均深入到陶瓷复合材料中，此过程中会在陶瓷复合材料的表层形成氮化碳、氮化硅(偶联剂中含有Si)、碳化硅等超硬物质，增加陶瓷复合材料的硬度，进一步提高耐磨性。
具体实施方式
现在结合实施例对本发明作进一步详细的说明。
人工关节用陶瓷复合材料的制备方法如下：
(1)按比例称取各组分，加入去离子水，搅拌均匀配成浆料，然后在球磨机中对上述浆料进行球磨，得到分散均匀的浆料；
(2)对步骤(1)中分散均匀的浆料进行喷雾干燥，得到造粒料；
(3)将步骤(2)中的造粒料冷压成型；
(4)将步骤(3)中的成型品放入模具中，在真空下或惰性气体保护下进行高温煅烧，煅烧温度为1100-1300℃，时间为1-5h，然后待自然冷却取出即可。
在具体的实施方式中，根据实际需求，也可以用硅烷偶联剂KH550对氧化铝、氧化锆、氧化铝纤维、氧化锌、氧化钙或氧化镁进行改性，一方面可以增加各种粉体材料的分散均匀性，另一方面可以增加偶联剂的含量，从而增加渗碳层和渗氮层的厚度，进一步增加所制备陶瓷复合材料的韧性和耐磨性。
硅烷偶联剂KH550改性氧化铝纤维的制备方法为：取720g乙醇和80g水配成醇水溶液，将200g硅烷偶联剂KH550加入其中，充分搅拌混合均匀，获得硅烷偶联剂水解液，将氧化铝纤维分散于水解液中，搅拌或超声震荡30-60min，过滤，干燥即可。
实施例1-7及对比例1-4各组分及其重量份用量以及具体工艺参数详见表1。
对于上述实施例和对比例中所制备的陶瓷复合材料进行性能测试，测试结果如下：
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (7)
1.一种人工关节用陶瓷复合材料，其特征在于：由以下重量份的各组分组成：氧化铝60-90份、氧化锆10-30份、氧化铝纤维3-10份、氧化锌0-2份、氧化钙0-5份、氧化镁0-5份；
所述人工关节用陶瓷复合材料的制备方法，包括如下步骤：
（1）按比例称取各组分，加入去离子水，搅拌均匀配成浆料，然后在球磨机中对上述浆料进行球磨，得到分散均匀的浆料；
（2）对步骤（1）中分散均匀的浆料进行喷雾干燥，得到造粒料；
（3）将步骤（2）中的造粒料冷压成型；
（4）将步骤（3）中的成型品放入模具中，在真空下或惰性气体保护下进行高温煅烧，煅烧温度为1100-1300℃，时间为1-5h，然后待自然冷却取出即可；
所述步骤（1）所用的氧化铝纤维为经硅烷偶联剂KH550改性氧化铝纤维。
2.如权利要求1所述的人工关节用陶瓷复合材料，其特征在于：所述氧化锆中含有氧化铪杂质，所述氧化铪杂质含量占氧化锆总质量的5%以下。
3.如权利要求1所述的人工关节用陶瓷复合材料，其特征在于：由以下重量份的各组分组成：氧化铝70-80份、氧化锆15-25份、氧化铝纤维5-8份、氧化锌0-2份、氧化钙0-5份、氧化镁0-5份。
4.如权利要求1所述的人工关节用陶瓷复合材料，其特征在于：所述氧化锆为氧化钇稳定的氧化锆。
5.如权利要求1所述的人工关节用陶瓷复合材料的制备方法，其特征在于：所述步骤（4）中高温煅烧的时间为3-5h。
6.如权利要求1所述的人工关节用陶瓷复合材料的制备方法，其特征在于：所述步骤（1）中去离子水与各组分总量的质量比为2:1-1.5。
7.如权利要求1所述的人工关节用陶瓷复合材料的制备方法，其特征在于：所述步骤（1）中球磨过程中的料球比为1:0.5-1.5。
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