CN109536804B - 钽合金、类金刚石碳镀层钽合金和类金刚石碳镀层生物医学植入用钽合金骨爪及其制备方法 - Google Patents

钽合金、类金刚石碳镀层钽合金和类金刚石碳镀层生物医学植入用钽合金骨爪及其制备方法 Download PDF

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CN109536804B
CN109536804B CN201811480776.2A CN201811480776A CN109536804B CN 109536804 B CN109536804 B CN 109536804B CN 201811480776 A CN201811480776 A CN 201811480776A CN 109536804 B CN109536804 B CN 109536804B
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tantalum alloy
diamond
carbon coating
claw
bone
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陶军晖
吴田
戴伟
胡锋
邱尚焜
王昊
周雨娟
张玲玲
万哲言
汪翠柳
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Hubei University of Education
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Abstract

本发明公开了一种钽合金和一种类金刚石碳镀层生物医学植入用钽合金骨爪及其制备方法。本发明的钽合金，包括如下质量百分数的组分：Al:5～6％，Zn:3～4％,Ga:3～4％，Y:2～3％，Si:1～2％，Mg:1～2％，其余为Ta及不可避免的杂质。一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，包括如下步骤：进行等离子体化学气相沉积在骨爪表面沉积一层类金刚石碳镀层等。本发明采用等离子体化学气相沉积的方法，在生物医学植入用钽合金骨爪表面形成了一层致密类金刚石碳镀层根本上解决了腐蚀问题，又能够增加钽合金与骨头界面的结合力，防止两者之间产生滑移，为人体骨骼修复提供了安全可靠的生物医学植入连接器件。

Description

钽合金、类金刚石碳镀层钽合金和类金刚石碳镀层生物医学 植入用钽合金骨爪及其制备方法
技术领域
本发明涉及生物医学技术领域，尤其涉及一种钽合金、类金刚石碳镀层钽合金和类金刚石碳镀层生物医学植入用钽合金骨爪及其制备方法。
背景技术
钽合金具有熔点高、蒸汽压低、冷加工性能好、化学稳定性高等优点，可用于制造生物医学植入用骨爪。在人体的服役环境中，大量的酸性物质会腐蚀钽合金基体，使其结合强度降低，同时在循环应力的作用下导致其最终开裂。同时，钽合金骨爪与骨头(主要成分为羟基磷灰石)的接触界面也会出现结合不牢出现滑移的情况。近年来，随着钽合金骨爪在生物医学植入领域中的大量应用，骨爪与骨头界面产生滑移的频发造成了大量骨折断裂的严重问题，为了保证生物医学植入用钽合金骨爪的安全可靠性，急需开发出一种既能够进一步增加钽合金抗腐蚀性能，又能够抵抗钽合金与骨头界面产生滑移的生物医学植入用钽合金骨爪。
目前，为了使生物医学植入用钽合金骨爪在人体酸性环境下避免进一步腐蚀，又提高骨爪与骨头界面的结合力，本发明通过等离子体化学气相沉积在常规钽合金骨爪表面附着一层致密的类金刚石碳镀层。类金刚石碳镀层具有高硬度、高耐磨损、低摩擦系数、高耐腐蚀、组织相容和血液相容的优良特性，可极大地提高钽合金骨爪的耐腐蚀性能，同时该类金刚石碳镀层与骨头中的羟基磷灰石具有较好的相容结合性，可大大提高骨爪与骨头的界面结合力。这种类金刚石碳镀层使生物医学植入用钽合金骨爪从根本上解决了腐蚀问题，又能够防止钽合金与骨头界面产生滑移。
发明内容
本发明的目的在于，针对现有技术的上述不足，提出一种钽合金和一种类金刚石碳镀层生物医学植入用钽合金骨爪及其制备方法。
本发明的一种类金刚石碳镀层生物医学钽合金，其特征在于：包括如下质量百分数的组分：Al:5～6％，Zn:3～4％，Ga:3～4％，Y:2～3％，Si:1～2％，Mg:1～2％，其余为Ta及不可避免的杂质。
一种类金刚石碳镀层钽合金，由上述的钽合金进行等离子体化学气相沉积在其表面沉积一层类金刚石碳镀层制得。
本发明的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：包括如下步骤：
1)制备权利要求1所述的钽合金
2)采用切割机和机床将所述钽合金板加工成单个的骨爪；
3)对骨爪表面进行常规喷丸，使钽合金骨爪表面无氧化层残留；喷丸可提高钽合金骨爪表面类金刚石碳镀层的密着性能；
4)进行常规电解脱脂；脱脂可去掉钽合金骨爪表面油脂，也有利于增加类金刚石碳镀层的密着性能；
5)进行等离子体化学气相沉积在骨爪表面沉积一层类金刚石碳镀层；
6)进行风冷、水洗并烘干，消毒风干、无菌包装后出货。
优选的，步骤5)中等离子体化学气相沉积的放电功率4～5W，基体温度200～250℃，反应压力90～100Pa，气体流量30～40mL/min。
优选的，步骤1)包括如下步骤：
a)经混合原料、压制成熔炼电极、熔炼电极和残料焊接成自耗电极、合金化熔炼、浇注成板坯；
b)将板坯加热后进行粗轧和精轧，然后冷却后卷取得钽合金材料。
优选的，步骤a)中的合金化熔炼采用真空自耗熔炼炉进行熔炼，熔炼温度2100～2200℃。
优选的，步骤b)中加热温度在1600～1700℃，均热时间为110～120min；粗轧结束温度不低于1400℃；控制精轧结束温度在950～1000℃。
优选的，步骤b)中的冷却进行的是层流冷却，采用在线淬火方式，终冷温度为350～400℃，冷却速度：53～56℃/s。
优选的，步骤1)中制备的所述钽合金的力学性能达到屈服强度ReL:≥500MPa，抗拉强度Rm≥700MPa，延伸率A≥25％。
本发明的一种类金刚石碳镀层生物医学植入用钽合金骨爪，其特征在于：由权利要求2-7所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法制备。
本发明采用等离子体化学气相沉积的方法，在生物医学植入用钽合金骨爪表面形成了一层致密类金刚石碳镀层；生物医学植入用钽合金骨爪表面所形成的致密类金刚石碳镀层使生物医学植入用钽合金骨爪从根本上解决了腐蚀问题，又能够增加钽合金与骨头界面的结合力，防止两者之间产生滑移，为人体骨骼修复提供了安全可靠的生物医学植入连接器件。
具体实施方式
以下是本发明的具体实施例对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例。
采用如下步骤制备：本发明的类金刚石碳镀层生物医学植入用钽合金骨
1)采用真空自耗熔炼炉进行钽合金的熔炼，经混合金料、压制电极、电极和残料焊接成自耗电极、合金化熔炼(熔炼温度2100～2200℃)、浇注成板坯；
2)将板坯加热，加热温度在1600～1700℃，均热时间为110～120min；
3)进行粗轧，并控制粗轧结束温度不低于1400℃；
4)进行精轧，并控制终轧温度在950～1000℃；
5)进行层流冷却，采用在线淬火方式，终冷温度为350～400℃，冷却速度：53～56℃/s；
6)进行卷取，制得热轧板卷；
7)精整切边：按标准规格切取钽合金板，并切除钽板周围毛边，切割余量5～10mm；
8)采用切割机和机床将钽合金板加工成单个的骨爪；
9)对骨爪表面进行常规喷丸，使钽合金骨爪表面无氧化层残留；
10)进行常规电解脱脂；
11)进行等离子体化学气相沉积在骨爪表面沉积一层类金刚石碳镀层，放电功率4～5W，基体温度200～250℃，反应压力90～100Pa，气体流量30～40ml/min；
12)进行风冷、水洗并烘干。
13)消毒风干、无菌包装后出货。
表1本发明各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪化学成分
实施例 Al Zn Ga Y Si Mg Ta
1 6.0 4.0 3.0 2.0 1.0 2.0 82.0
2 5.1 3.9 3.5 2.2 1.2 1.9 82.2
3 5.9 3.1 4.0 2.5 1.5 1.1 81.9
4 5.6 3.4 3.7 3.0 2.0 1.0 81.3
5 5.0 3.6 3.9 2.9 1.9 1.3 81.4
6 5.3 3.0 3.1 2.7 1.8 1.5 82.6
表2本发明各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪熔炼工艺
实施例 熔炼温度(℃)
1 2110
2 2200
3 2150
4 2190
5 2100
6 2170
表3本发明各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪轧制工艺
Figure BDA0001893327660000051
表4本发明各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪等离子体化学气相沉积工艺
Figure BDA0001893327660000061
表5本发明各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪力学性能
Figure BDA0001893327660000062
表6本发明各实施例的各实施例的类金刚石碳镀层生物医学植入用钽合金骨爪的耐腐蚀性能和抗疲劳性能
Figure BDA0001893327660000071
从表5和表6中可以看出，本发明申请的类金刚石碳镀层生物医学植入用钽合金骨爪，其屈服强度为500～541MPa，抗拉强度为700～730MPa，延伸率为25～27％；耐腐蚀性能(96h腐蚀失重量0.11～0.21mg/cm2)均远远高于对比例Ta合金(96h腐蚀失重量1.73mg/cm2)；在同样条件下，置氢疲劳寿命(71258～74128次)远远高于对比例Ta合金(17356次)。产品性能完全满足使用要求，并且其耐腐蚀性能和抗疲劳寿命远远优于对比例Ta合金。以上未涉及之处，适用于现有技术。
虽然已经通过示例对本发明的一些特定实施例进行了详细说明，但是本领域的技术人员应该理解，以上示例仅是为了进行说明，而不是为了限制本发明的范围，本发明所属技术领域的技术人员可以对所描述的具体实施例来做出各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的方向或者超越所附权利要求书所定义的范围。本领域的技术人员应该理解，凡是依据本发明的技术实质对以上实施方式所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围。

Claims (9)

1.一种类金刚石碳镀层钽合金，其特征在于：由钽合金进行等离子体化学气相沉积在其表面沉积一层类金刚石碳镀层制得；
其中，所述钽合金包括如下质量百分数的组分：Al:5～6％，Zn:3～4％,Ga:3～4％，Y:2～3％，Si:1～2％，Mg:1～2％，其余为Ta及不可避免的杂质。
2.一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：包括如下步骤：
1)制备如权利要求1所述的钽合金；
2)采用切割机和机床将所述钽合金加工成单个的骨爪；
3)对骨爪表面进行常规喷丸，使钽合金骨爪表面无氧化层残留；
4)进行常规电解脱脂；
5)进行等离子体化学气相沉积在骨爪表面沉积一层类金刚石碳镀层；
6)进行风冷、水洗并烘干，消毒风干、无菌包装后出货。
3.如权利要求2所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤5)中等离子体化学气相沉积的放电功率4～5W，基体温度200～250℃，反应压力90～100Pa，气体流量30～40mL/min。
4.如权利要求3所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤1)包括如下步骤：
a)经混合原料、压制成熔炼电极、熔炼电极和残料焊接成自耗电极、合金化熔炼、浇注成板坯；
b)将板坯加热后进行粗轧和精轧，然后冷却后卷取得钽合金材料。
5.如权利要求4所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤a)中的合金化熔炼采用真空自耗熔炼炉进行熔炼，熔炼温度2100～2200℃。
6.如权利要求5所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤b)中加热温度在1600～1700℃，均热时间为110～120min；粗轧结束温度不低于1400℃；控制精轧结束温度在950～1000℃。
7.如权利要求6所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤b)中的冷却进行的是层流冷却，采用在线淬火方式，终冷温度为350～400℃，冷却速度：53～56℃/s。
8.如权利要求2-7任一项所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法，其特征在于：步骤(1)中制备的所述钽合金的力学性能达到屈服强度ReL:≥500MPa，抗拉强度Rm≥700MPa，延伸率A≥25％。
9.一种类金刚石碳镀层生物医学植入用钽合金骨爪，其特征在于：由权利要求2-7所述的一种类金刚石碳镀层生物医学植入用钽合金骨爪的制备方法制备得到。
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