CN111850497A - 一种纳米二氧化钛覆膜根管锉及其制备方法 - Google Patents
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Abstract
本发明涉及生物医用金属制品领域，尤其涉及一种纳米二氧化钛覆膜根管锉及其制备方法。一种纳米二氧化钛覆膜根管锉，以镍钛形状记忆合金为基体，其表面制备纳米二氧化钛覆膜，厚度为60‑100nm。本发明提供的纳米二氧化钛覆膜根管锉采用NiTi形状记忆合金具有生物功能性，其力学性能适用于人体；其表面纳米二氧化钛覆膜具有生物陶瓷的生物相容性，无毒性，具有良好的生物安全性，具有很大的优势和应用前景。本发明提供的纳米二氧化钛覆膜根管锉制备方法中采用的覆膜方法工艺简单，但覆膜效果好。本发明提供的纳米二氧化钛覆膜根管锉在医学上使用安全、实用性好。
Description
技术领域
本发明涉及生物医用金属制品领域，尤其涉及一种纳米二氧化钛覆膜根管锉及其制备方法。
背景技术
齿科用的锉多为医用奥氏体不锈钢，通常以镍作为主要奥氏体化元素(如316L、317L 等)，含镍量约在14％左右。研究及临床统计表明，镍会引起一些人的过敏反应，甚至致畸和引起癌变。随着研究的深入，镍对人体的毒害作用愈来愈受到重视。
316L和317L型不锈钢是广泛使用的金属生物材料，目前已在齿科大批量应用的根管锉即由此类材料制成。近年来开始使用镍钛形状记忆合金制造这类根管锉，利用镍钛合金的形状记忆效应和超弹性，以及耐疲劳耐腐蚀等特性，可以使根管锉随着牙根的形状进行各种弯曲而不会折断，从而减少医疗事故，增加根管治疗的成功率，使患者减轻痛苦，给医生带来方便。但是镍钛形状记忆合金在制造根管锉的的过程中，由于金属韧性的需求，导致强度和耐磨性不足，清理根管不干净；同时，镍钛形状记忆合金也包含50％(名义成分)的镍，同样有镍离子析出导致毒性过敏现象。
鉴于以上情况，对镍钛合金根管锉表面改性涂层是必要的。钛及钛合金具有良好的耐蚀性和生物相容性，主要因为其表面存在非常稳定的氧化膜。钛和氧的亲和力很强，在含氧的环境中可在表面迅速形成稳定的二氧化钛氧化膜，使其表现出很好的耐蚀性。钛表面氧化膜的主要优点是：①二氧化钛具有较低的固有毒性；②二氧化钛在水中的溶解度很低；③钛阳离子与生物分子的反应活性很低，接近化学惰性；④过氧化物化学性能具有明显的抗炎作用。二氧化钛薄膜对镍钛形状记忆合金进行表面改性可提高其耐腐蚀性能和血液相容性，防止镍离子析出。
镍钛形状记忆合金的超弹性的可恢复变形为8-10％，作为生物陶瓷的二氧化钛几乎没有塑性。因此，改性二氧化钛的性能以适应基体镍钛合金的超弹性是重要的环节，不但能使镍钛形状记忆合金的生物功能性及生物相容性得到很好的应用。表面覆膜纳米化后，性能得到了改善，可以适应基础材料的使用性能。
发明内容
针对上述问题，本发明提供一种纳米二氧化钛覆膜根管锉及其制备方法。所述根管锉组成材料为既具有生物相容性又有生物功能性的镍钛形状记忆合金，其表面覆有纳米二氧化钛膜，以改善镍钛合金基体的镍离子析出问题，提高耐磨性，同时具有良好的生物相容性。
为了实现上述目的，本发明采用以下技术方案。
一种纳米二氧化钛覆膜根管锉，以镍钛形状记忆合金为基体，其表面制备纳米二氧化钛覆膜，厚度为60-100nm。
进一步地，所述镍钛形状记忆合金为生物医用镍钛形状记忆合金，是由以下质量分数的成分组成：镍50-51％，余量为钛；材料的杂质含量：氧＜300ppm，氮＜30ppm。
一种纳米二氧化钛覆膜根管锉的制备方法，具体包括以下步骤。
步骤1、通过活化溅射覆膜方法获得纳米二氧化钛膜，该方法在真空状态下进行，采用偏压磁控溅射工艺，通氧活化镍钛合金根管锉表面，使其自身钛与氧化合，产生致密二氧化钛氧化膜。
步骤2、同时采用高速电子溅射纯金属钛源，活化的钛与活化氧在空中化合过程中沉积于基体表面，得到加固复合膜层，厚度为60-100nm。
进一步地，所述步骤1中的环境温度控制在300-400℃。
进一步地，所述步骤2中的环境温度控制在300-400℃。
与现有技术比，本发明的有益效果如下。
(1)本发明提供的纳米二氧化钛覆膜根管锉生物功能性好，采用超纯冶炼的二元镍钛形状记忆合金，具有准确的马氏体转变温度，气体含量低，材料的工艺性能好。因此，可以保证材料具有良好的超弹性和温度记忆效应。
(2)本发明提供的纳米二氧化钛覆膜根管锉生物相容性好，采用二氧化钛纳米膜，具有良好的生物相容性，改变了陶瓷的脆性，与基体获得了同样的生物功能性。致密的覆膜阻挡了镍离子的析出，保证了NiTi形状记忆合金的生物相容性。
(3)本发明提供的纳米二氧化钛覆膜根管锉在医学上使用安全、实用性好。NiTi形状记忆合金的生物功能性，力学性能适用于人体。而TiO2的生物陶瓷的生物相容性，无毒性，具有良好的生物安全性，具有很大的优势和应用前景。
(4)本发明提供的纳米二氧化钛覆膜根管锉制备方法中采用的覆膜方法工艺简单， 但覆膜效果好。
具体实施方式
下面结合具体实施例对本发明做详细的说明。
实施例1。
一种纳米二氧化钛覆膜根管锉，以镍钛形状记忆合金为基体，其表面制备纳米二氧化钛覆膜，厚度为60-100nm。
进一步地，所述镍钛形状记忆合金为生物医用镍钛形状记忆合金，是由以下质量分数的成分组成：镍50-51％，余量为钛，材料的杂质含量：氧＜300ppm，氮＜30ppm。
所述镍钛形状记忆合金为超纯冶炼制取，具体制备方法包括以下步骤。
步骤1、选择高温稳定性的坩埚CaO坩埚，使其在冶炼过程中不能被高还原性的Ti所还原，形成Ti的氧化物而影响成分的比例，同时，由于Ni和Ti的比例准确而获得准确地设计成分，得到稳定相变温度的NiTi形状记忆合金。
步骤2、采用分段控制、真空熔炼、惰性气体保护下的熔炼工艺，能确保外界带来的杂质不被引入，也由于在惰性气体的保护下熔炼及浇注，防止喷溅以保证成分准确。
步骤3、利用合金化和防热进行下阶段反应，防止过热产生Ti的氧化。
一种纳米二氧化钛覆膜根管锉的制备方法，具体包括以下步骤。
步骤1、通过活化溅射覆膜方法获得纳米二氧化钛膜，该方法在真空状态下进行，环境温度控制在300-400℃，采用偏压磁控溅射工艺，通氧活化镍钛合金根管锉表面，使其自身钛与氧化合，产生致密二氧化钛氧化膜。
步骤2、同时采用高速电子溅射纯金属钛源，活化的钛与活化氧在空中化合过程中沉积于基体表面，使用温度300-400℃，得到加固复合膜层，厚度60-100nm。
制得纳米二氧化钛覆膜根管锉检测结果见表1，二氧化钛氧化膜与基体结合紧密，保 持基体的力学性能，表面光洁，超弹性变形中无裂纹及脱落。完全适应大变形的基体镍钛合 金的8-10％的可恢复变形，无生物毒性。
表1纳米二氧化钛覆膜根管锉性能检测结果。
Claims (5)
1.一种纳米二氧化钛覆膜根管锉，其特征在于，所述根管锉是以镍钛形状记忆合金为基体，其表面制备纳米二氧化钛覆膜，厚度为60-100nm。
2.如权利要求1所述的纳米二氧化钛覆膜根管锉，其特征在于，所述镍钛形状记忆合金为生物医用镍钛形状记忆合金，是由以下质量分数的成分组成：镍50-51％，余量为钛；材料的杂质含量：氧＜300ppm，氮＜30ppm。
3.如权利要求1所述的纳米二氧化钛覆膜根管锉的制备方法，其特征在于，具体包括以下步骤：
步骤1、通过活化溅射覆膜方法获得纳米二氧化钛膜，该方法在真空状态下进行，采用偏压磁控溅射工艺，通氧活化镍钛合金根管锉表面，使其自身钛与氧化合，产生致密二氧化钛氧化膜；
步骤2、同时采用高速电子溅射纯金属钛源，活化的钛与活化氧在空中化合过程中沉积于基体表面，得到加固复合膜层，厚度为60-100nm。
4.如权利要求3所述的纳米二氧化钛覆膜根管锉的制备方法，其特征在于，所述步骤1中的环境温度控制在300-400℃。
5.如权利要求3所述的纳米二氧化钛覆膜根管锉的制备方法，其特征在于，所述步骤2中的环境温度控制在300-400℃。
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