CN108166040A - 一种Ta2O5/TiO2/3D多孔钛材料及制备方法 - Google Patents

一种Ta2O5/TiO2/3D多孔钛材料及制备方法 Download PDF

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CN108166040A
CN108166040A CN201711365746.2A CN201711365746A CN108166040A CN 108166040 A CN108166040 A CN 108166040A CN 201711365746 A CN201711365746 A CN 201711365746A CN 108166040 A CN108166040 A CN 108166040A
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王辉
李广忠
杨伟刚
向长淑
朱纪磊
贾文鹏
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Xi'an Sailong Additive Technology Co ltd
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Abstract

本发明公开了一种Ta2O5/TiO2/3D多孔钛材料及制备方法，涉及复合金属多孔材料制备技术领域。制备方法包括：对3D多孔钛进行抛光，将抛光后的所述3D多孔钛放入柠檬酸钠基溶液内进行阳极氧化处理，将阳极氧化处理后的所述3D多孔钛浸渍到钽涂液中，对浸渍后的所述3D多孔钛进行烘干，并将烘干后的所述3D多孔钛放入马弗炉中进行烧结。

Description

一种Ta2O5/TiO2/3D多孔钛材料及制备方法
技术领域
本发明涉及复合金属多孔材料制备技术领域，更具体的涉及一种 Ta2O5/TiO2/3D多孔钛材料及制备方法。
背景技术
钛合金材料由于其比强度高、易加工成形、原料资源丰富且生物相容性良 好等特点，目前已发展成为外科植入物普遍应用的功能结构材料。然而，复杂 的人体内环境会引起钛合金材料腐蚀而导致有毒元素的释放，相应的会降低生 物相容性；而且，钛合金的弹性模量与人体骨组织相差较大，易产生应力屏蔽 效应。需要寻求更耐腐蚀、生物相容性更佳、与人骨力学性能更为接近的新型 金属植入材料。
金属钽(Ta)材料具有优异的耐腐蚀性和优异的生物相容性，目前受到越 来越多的医学和材料科学工作者的关注，但其高昂的原料成本制约了其在生物 医用领域的广泛应用。
发明内容
本发明实施例所要解决的技术问题在于针对现有技术的不足，提供了一种 Ta2O5/TiO2/3D多孔钛材料制备方法。
本发明实施例提供了一种Ta2O5/TiO2/3D多孔钛材料，所述材料由上至下 包括：Ta2O5涂层，TiO2过渡层以及3D多孔钛基体。
优选地，所述Ta2O5涂层的厚度介于5～15μm。
优选地，所述TiO2过渡层的厚度介于0.5～1.5μm。
本发明实施例还提供一种Ta2O5/TiO2/3D多孔钛材料的制备方法，包括：
对3D多孔钛进行抛光，其中，所述3D多孔钛进行抛光采用配比为： VOL1％HF+VOL3％HNO3的电解液，抛光时间介于15～25min；
将抛光后的所述3D多孔钛放入柠檬酸钠基溶液内进行阳极氧化处理，阳 极氧化处理时间介于30～120min；
将阳极氧化处理后的所述3D多孔钛浸渍到钽涂液中，浸渍时间介于 10～15min，对浸渍后的所述3D多孔钛进行烘干，并将烘干后的所述3D多孔 钛放入马弗炉中，当所述马弗炉1℃/min的升温速度到450℃～600℃后，将所 述3D多孔钛在所述马弗炉保温90～150min。
优选地，所述钽涂液中水与钽的比例为：3～5:1。
优选地，所述柠檬酸钠基溶液包括45～60g/L C4H4O6·Na2·2H2O，150～200g/LNaOH，30g/L C10H16N2O8和6g/LNaSiO3·9H2O。
优选地，所述阳极氧化处理时的电压介于10～60V，电流密度为5～8 A/dm2。
本发明实施例中，提供了一种Ta2O5/TiO2/3D多孔钛材料的制备方法，包 括：对3D多孔钛进行抛光，其中，所述3D多孔钛进行抛光采用配比为： VOL1％HF+VOL3％HNO3的电解液，抛光时间介于15～25min；将抛光后的所 述3D多孔钛放入柠檬酸钠基溶液内进行阳极氧化处理，阳极氧化处理时间介 于30～120min；将阳极氧化处理后的所述3D多孔钛浸渍到钽涂液中，浸渍时 间介于10～15min，对浸渍后的所述3D多孔钛进行烘干，并将烘干后的所述 3D多孔钛放入马弗炉中，当所述马弗炉1℃/min的升温速度到450℃～600℃后， 将所述3D多孔钛在所述马弗炉保温90～150min。上述制备方法中，采用电化 学抛光+阳极氧化+涂层烧结技术，制备的Ta2O5/TiO2/3D多孔钛材料不仅具有 钛合金的优点，且兼具Ta2O5的更高的生物相容性。解决了钛合金骨植入时复 杂的人体内环境引起钛合金材料腐蚀而导致有毒元素的释放，降低其生物相容 性，并引起细胞中毒的问题；进一步地，以3D多孔钛为基体，实现了钽材料 在生物植入方面的低成本应用，大大拓宽了其应用领域。
具体实施方式
下面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，都属于本发明保护的范围。
本发明实施例提供了一种Ta2O5/TiO2/3D多孔钛材料，该材料由上至下依 此包括Ta2O5涂层，TiO2过渡层和3D多孔钛基体。
具体地，Ta2O5涂层的厚度介于5～15μm；TiO2过渡层的厚度介于 0.5～1.5μm。
基于上述Ta2O5/TiO2/3D多孔钛材料，可以通过下列介绍的制备方法，来 具体制备Ta2O5/TiO2/3D多孔钛。
实施例1
步骤一、采用电化学抛光工艺进行3D多孔钛的抛光，其中，3D多孔钛由 电子束3D打印制备，3D打印的多孔钛的尺寸为30×30×30mm3。在实际应用 中，电化学抛光液为VOL1％HF+VOL3％HNO3，电压为0.5V，电解抛光时间 20min；
步骤二、在柠檬酸钠基溶液中，进行3D多孔钛阳极氧化处理，其中，电 压为40V，阳极氧化处理时间60min；
步骤三、将0.015mol的乙醇钽溶解到无水乙醇中，然后缓慢加入水，水与 钽的比例为：3:1，制备成钽涂液；
步骤四、将阳极氧化后的多孔钛浸渍到钽涂液中，保持10min,然后以 0.5mm/s的速度取出，然后在40℃温度条件下，缓慢烘干；
步骤五、将烘干后的样品放置到马弗炉中，以1℃/min的升温速度到450℃， 保温2小时。
实施例2
步骤一、采用电化学抛光工艺进行3D多孔钛的抛光，其中，3D多孔钛由 电子束3D打印制备，3D打印的多孔钛尺寸为Φ50×30mm3。在实际应用中， 电化学抛光液为VOL1％HF+VOL3％HNO3，电压为1.8V，电解抛光时间20min；
步骤二、在柠檬酸钠基溶液中，进行3D多孔钛阳极氧化处理，电压20V, 时间60min；
步骤三、将0.025mol的乙醇钽溶解到无水乙醇中，然后缓慢加入水，水与 钽的比例为：5:1，制备成钽涂液；
步骤四、将阳极氧化后的多孔钛浸渍到钽涂液中，保持10min,然后以 1mm/s的速度取出，然后在30℃温度条件下，缓慢烘干；
步骤五、将烘干后的样品放置到马弗炉中，以1℃/min的升温速度到600℃， 保温2小时。
综上所述，本发明实施例中提供了一种Ta2O5/TiO2/3D多孔钛材料的制备 方法，采用电化学抛光+阳极氧化+涂层烧结技术，制备的Ta2O5/TiO2/3D多孔 钛材料不仅具有钛合金的优点，且兼具Ta2O5的更高的生物相容性。解决了钛 合金骨植入时复杂的人体内环境引起钛合金材料腐蚀而导致有毒元素的释放， 降低其生物相容性，并引起细胞中毒的问题；进一步地，以3D多孔钛为基体， 实现了Ta涂层的低成本应用，大大拓宽了其应用领域。
尽管已描述了本发明的优选实施例，但本领域内的技术人员一旦得知了基 本创造性概念，则可对这些实施例作出另外的变更和修改。所以，所附权利要 求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
显然，本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发 明的精神和范围。这样，倘若本发明的这些修改和变型属于本发明权利要求及 其等同技术的范围之内，则本发明也意图包含这些改动和变型在内。

Claims (7)

1.一种Ta2O5/TiO2/3D多孔钛材料，其特征在于，所述材料由上至下包括：Ta2O5涂层，TiO2过渡层以及3D多孔钛基体。
2.如权利要求1所述的Ta2O5/TiO2/3D多孔钛材料，其特征在于，所述Ta2O5涂层的厚度介于5～15μm。
3.如权利要求1所述的Ta2O5/TiO2/3D多孔钛材料，其特征在于，所述TiO2过渡层的厚度介于0.5～1.5μm。
4.一种Ta2O5/TiO2/3D多孔钛材料的制备方法，其特征在于，包括：
对3D多孔钛进行抛光，其中，所述3D多孔钛进行抛光采用配比为：VOL1％HF+VOL3％HNO3的电解液，抛光时间介于15～25min；
将抛光后的所述3D多孔钛放入柠檬酸钠基溶液内进行阳极氧化处理，阳极氧化处理时间介于30～120min；
将阳极氧化处理后的所述3D多孔钛浸渍到钽涂液中，浸渍时间介于10～15min，对浸渍后的所述3D多孔钛进行烘干，并将烘干后的所述3D多孔钛放入马弗炉中，当所述马弗炉1℃/min的升温速度到450℃～600℃后，将所述3D多孔钛在所述马弗炉保温90～150min。
5.如权要求4所述的制备方法，其特征在于，所述钽涂液中水与钽的比例为：3～5:1。
6.如权利要求4所述的制备方法，其特征在于，所述柠檬酸钠基溶液包括45～60g/LC4H4O6·Na2·2H2O，150～200g/L NaOH，30g/L C10H16N2O8和6g/L NaSiO3·9H2O。
7.如权利要求4所述的制备方法，其特征在于，所述阳极氧化处理时的电压介于10～60V，电流密度为5～8A/dm2。
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