CN114657561A - 一种具有疏水表面改性涂层的射频消融针及其制备方法 - Google Patents
一种具有疏水表面改性涂层的射频消融针及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有疏水表面改性涂层的射频消融针及其制备方法，包括本体，所述本体表面设有过渡层，所述过渡层表面设有导电疏水层；其中，所述过渡层通过PVD沉积形成，所述导电疏水层通过PECVD沉积形成。本发明通过在非晶碳膜中掺杂铬和氟原子，来改性射频消融针针尖表面。其中，非晶碳膜具有良好的生物相容性和低摩擦系数；铬的掺杂提高了非晶碳膜的导电性能，因而能增大恶性肿瘤的消融范围，增强消融治疗的效果；而氟的掺杂提高了非晶碳膜的疏水性，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，从而减少组织阻抗和提高导电性，满足消融针更高的使用要求。
Description
技术领域
本发明属于医疗设备技术领域，涉及一种射频消融针，特别涉及一种具有高导电、低摩擦和高疏水性表面改性涂层的射频消融针及其制备方法。
背景技术
射频消融治疗(Radio frequency Ablation,RFA)是不可切除的肝脏肿瘤的首选局部消融技术之一。其基本原理是460-500kHz的射频波产生摩擦热，通过热传导从电极分布到组织中。在接近或大于60℃的温度下，细胞损伤变得不可逆转：细胞内蛋白质和胶原蛋白变性，脂质溶解，并发生细胞坏死。实验研究表明，传递到组织中的能量越多，局部达到的温度越高，产生的消融区域越大，消融越完整。然而，在射频消融过程中容易发生针尖与周围组织的粘连，这大大增加了电极周围发生炭化的几率，从而增加了组织阻抗和降低了导电性，因此使得将能量有效地传递到深层组织变得更加困难。另外，由于射频消融针表面粗糙，摩擦阻力大，消融过程中容易引发细菌感染、气胸等并发症。
非晶碳膜是一种可以用于医学领域的且具有优异性能的薄膜材料，在生物医学等领域有着非常宽广的发展前景。例如，在用于人工器官瓣膜的不锈钢表面沉积类金刚石薄膜，可以提高材料的耐磨擦耐腐蚀性能并使其能够更好地与人体结合。
但是，本征非晶碳薄膜的疏水性能较差，接触角大都在60°左右，很难满足射频消融针的疏水性要求。
发明内容
本发明的目的是为了解决现有本征非晶碳薄膜的疏水性能较差的缺陷而提供一种具有高导电、低摩擦和高疏水性表面改性涂层的射频消融针，通过在非晶碳膜中掺杂铬和氟原子，来改性射频消融针针尖表面。其中，非晶碳膜具有良好的生物相容性和低摩擦系数；铬的掺杂提高了非晶碳膜的导电性能，因而能增大恶性肿瘤的消融范围，增强消融治疗的效果；而氟的掺杂提高了非晶碳膜的疏水性，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，从而减少组织阻抗和提高导电性，满足消融针更高的使用要求。
为实现以上目的，本发明的技术方案通过以下技术方案予以实现：
一种具有疏水表面改性涂层的射频消融针，包括本体，所述本体表面设有过渡层，所述过渡层表面设有导电疏水层；其中，所述过渡层通过PVD沉积形成，所述导电疏水层通过PECVD沉积形成。
在本发明中，非晶碳膜具有良好的生物相容性和低摩擦系数，通过导电疏水层，提供导电性能以及疏水性能，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，从而减少组织阻抗和提高导电性，满足消融针更高的使用要求。
作为本发明的一种优选方案，所述过渡层为Cr金属层。
作为本发明的一种优选方案，所述导电疏水层为Cr/F共掺杂的非晶碳膜。
在本技术方案中，非晶碳膜是一种含有聚合氢的非晶体碳膜(a-C:H)，由于具有耐磨和低摩擦系数，而成为固体润滑薄膜材料，成分由SP3键合的四面体金刚石结构，SP2键合的平面石墨结构和聚合氢的混合构成。
通过在非晶碳膜中掺杂铬和氟原子，来改性射频消融针针尖表面，铬的掺杂提高了非晶碳膜的导电性能，因而能增大恶性肿瘤的消融范围，增强消融治疗的效果；而氟的掺杂提高了非晶碳膜的疏水性，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，从而减少组织阻抗和提高导电性。
作为本发明的一种优选方案，所述过渡层的厚度为50-500nm。
作为本发明的一种优选方案，所述的导电疏水层厚度为1-3μm。
本发明还提供了一种具有疏水表面改性涂层的射频消融针的制备方法，包括以下步骤：
S1：将射频消融针的针尖端超声清洗；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：设定条件，针尖通过氩气辉光放电预溅射以清洁和激活表面；
S4：通入氩气气体，调节参数；开启金属溅射靶，在基底上沉积过渡层；
S5：通入碳源和氟源气体，调节金属靶功率，沉积掺杂导电疏水层；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
作为本发明的一种优选方案，所述步骤S1中，清洗是将针尖端在丙酮和去离子水中超声清洗。
作为本发明的一种优选方案，所述步骤S3中，条件为在1.0Pa的气压与-900V的偏压。
作为本发明的一种优选方案，所述步骤S4中，参数为：沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。
作为本发明的一种优选方案，所述步骤S5中，碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合；氟源气体为四氟甲烷、六氟乙烷、八氟丙烷、四氟乙烯和六氟丙烯中的任意一种或其任何组合。
本发明提供一种高导电、低摩擦和高疏水性掺杂非晶碳膜的制备方法，与现有技术相比优点在于：
本发明使用具有高导电、低摩擦和高疏水性掺铬/氟的非晶碳膜改性射频消融针。其中，非晶碳膜具有良好的生物相容性和低摩擦系数；铬的掺杂提高了非晶碳膜的导电性能，因而能增大恶性肿瘤的消融范围，增强消融治疗的效果；而氟的掺杂提高了非晶碳膜的疏水性，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，降低气胸、血气胸等并发症的发生率，从而减少组织阻抗和提高导电性，满足消融针更高的使用要求。
附图说明
图1是本发明表面涂层的示意图。
图2是本发明实施例1和对比例1-3试样对水接触角图。
图中，1.本体；2.过渡层；3.导电疏水层。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面结合本发明实施例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作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。
参见图1，本发明提供了一种具有疏水表面改性涂层的射频消融针，包括本体1，所述本体1表面设有过渡层2，所述过渡层2表面设有导电疏水层3；其中，所述过渡层2通过PVD沉积形成，所述导电疏水层3通过PECVD沉积形成。
作为优选，过渡层2可以是Cr、Ti金属层及其合金中的一种。
作为选优，导电疏水层3为Cr/F共掺杂的非晶碳膜，薄膜表面粗糙度为5nm至20nm。
本发明为了得到具有高导电、低摩擦和高疏水性掺铬/氟的非晶碳膜改性射频消融针，过渡层2选择Cr。
实施例1：
本实施例提供了一种高导电、低摩擦和高疏水性的射频消融针的制备方法，所述非晶碳膜为含铬/氟的类金刚石碳薄膜，包括以下步骤：
S1：将射频消融针的针尖端在丙酮和去离子水中超声清洗10分钟；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：在1.0Pa的气压和-900V的偏压下，针尖通过氩气辉光放电预溅射(60sccm)持续20分钟以清洁和激活表面；
S4：通入氩气气体，调节偏置电压、靶功率、沉积温度和沉积气压等参数。先开启金属溅射靶，在基底上沉积Cr过渡层；
S5：通入碳源和氟源气体，调节Cr靶功率，沉积掺杂Cr/F的非晶碳膜导电疏水层；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
优选的，在本实施例中，所述步骤S5中形成掺Cr/F非晶碳膜的碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合。在本实施例中，碳源气体为乙炔。
优选的，步骤S5中形成掺Cr/F非晶碳膜的氟源气体为四氟甲烷、六氟乙烷、八氟丙烷、四氟乙烯和六氟丙烯中的任意一种或其任何组合。在本实施例中，氟源气体为四氟乙烯。
优选的，步骤S4中采用等离子体处理时腔室内的沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。在本实施例中，采用等离子体处理时腔室内的沉积气压范围为5Pa，偏置电压范围为-150V、沉积温度范围为200℃。
对比例1：
一种非晶碳膜的射频消融针的制备方法，包括以下步骤：
S1：将射频消融针的针尖端在丙酮和去离子水中超声清洗10分钟；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：在1.0Pa的气压和-900V的偏压下，针尖通过氩气辉光放电预溅射(60sccm)持续20分钟以清洁和激活表面；
S4：通入氩气气体，调节偏置电压、靶功率、沉积温度和沉积气压等参数。先开启金属溅射靶，在基底上沉积Cr过渡层；
S5：通入碳源气体，关闭Cr靶电源，沉积非晶碳膜；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
优选的，在本实施例中，所述步骤S5中形成非晶碳膜的碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合。在本对比例中，采用乙炔。
优选的，步骤S4中采用等离子体处理时腔室内的沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。在本对比例中，采用等离子体处理时腔室内的沉积气压范围为0.1Pa，偏置电压范围为-50V、沉积温度范围为25℃。
对比例2：
一种含铬的非晶碳膜的射频消融针的制备方法，包括以下步骤：
S1：将射频消融针的针尖端在丙酮和去离子水中超声清洗10分钟；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：在1.0Pa的气压和-900V的偏压下，针尖通过氩气辉光放电预溅射(60sccm)持续20分钟以清洁和激活表面；
S4：通入氩气气体，调节偏置电压、靶功率、沉积温度和沉积气压等参数。先开启金属溅射靶，在基底上沉积Cr过渡层；
S5：通入碳源气体，调节Cr靶功率，沉积掺杂Cr的非晶碳膜导电层；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
优选的，所述步骤S5中形成掺Cr非晶碳膜的碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合。在本对比例中，采用乙炔。
优选的，步骤S4中采用等离子体处理时腔室内的沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。在本对比例中，采用等离子体处理时腔室内的沉积气压范围为10Pa，偏置电压范围为-200V、沉积温度范围为500℃。
对比例3：
一种含氟非晶碳膜的射频消融针的制备方法，包括以下步骤：
S1：将射频消融针的针尖端在丙酮和去离子水中超声清洗10分钟；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：在1.0Pa的气压和-900V的偏压下，针尖通过氩气辉光放电预溅射(60sccm)持续20分钟以清洁和激活表面；
S4：通入氩气气体，调节偏置电压、靶功率、沉积温度和沉积气压等参数。先开启金属溅射靶，在基底上沉积Cr过渡层；
S5：通入碳源和氟源气体，关闭Cr靶电源，沉积掺F的非晶碳膜；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
优选的，所述步骤S5中形成掺F非晶碳膜的碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合。在本对比例中，碳源气体为甲烷。
优选的，所述步骤S5中形成掺F非晶碳膜的氟源气体为四氟甲烷、六氟乙烷、八氟丙烷、四氟乙烯和六氟丙烯中的任意一种或其任何组合。在本对比例中，氟源气体为四氟甲烷。
优选的，步骤S4中采用等离子体处理时腔室内的沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。在本对比例中，采用等离子体处理时腔室内的沉积气压范围为10Pa，偏置电压范围为-200V、沉积温度范围为500℃。
检测：
对上述实施例1和对比例1-3所得到的薄膜通过接触角测试仪分别进行接触角测试，结果如图2所示，可以看出，掺杂铬/氟的非晶碳膜(图2A)、纯非晶碳膜(图2B)、掺杂铬的非晶碳膜(图2C)和掺杂氟的非晶碳膜(图2D)对水的接触角分别是134°、61°、67°、102°。通过四探针电阻仪测试方阻来确定导电性，实施例1和对比例2的方阻均小于10-3Ω/□，对比例1的方阻是3.2*102Ω/□。通过球盘式摩擦试验机来测试薄膜摩擦系数，实施例1和不锈钢基底的摩擦系数分别是0.08、0.18。
综上所述，本发明所制备的掺铬/氟的非晶碳膜改性射频消融针表面，具有良好的生物相容性和低摩擦系数，提高了消融针的导电性能，因而能增大恶性肿瘤的消融范围，增强消融治疗的效果，而且提高了消融针表面的疏水性，减少针尖与周围组织的粘连，大大降低电极周围发生炭化的几率，从而减少组织阻抗和提高导电性，满足消融针更高的使用要求。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种具有疏水表面改性涂层的射频消融针，其特征在于，包括本体，所述本体的表面设有过渡层，所述过渡层的表面设有导电疏水层；其中，所述过渡层通过PVD沉积形成，所述导电疏水层通过PECVD沉积形成。
2.根据权利要求1所述的一种具有疏水表面改性涂层的射频消融针，其特征在于，所述过渡层为Cr金属层。
3.根据权利要求1所述的一种具有疏水表面改性涂层的射频消融针，其特征在于，所述导电疏水层为Cr/F共掺杂的非晶碳膜。
4.根据权利要求1所述的一种具有疏水表面改性涂层的射频消融针，其特征在于，所述过渡层的厚度为50-500nm。
5.根据权利要求1所述的一种具有疏水表面改性涂层的射频消融针，其特征在于，所述的导电疏水层厚度为1-3μm。
6.一种如权利要求1-5任一项所述的一种具有疏水表面改性涂层的射频消融针的制备方法，其特征在于，包括以下步骤：
S1：将射频消融针的针尖端超声清洗；
S2：将步骤S1中射频消融针的针尖放入真空室中，真空室抽真空，接通电源；
S3：设定条件，针尖通过氩气辉光放电预溅射以清洁和激活表面；
S4：通入氩气气体，调节参数；开启金属溅射靶，在基底上沉积过渡层；
S5：通入碳源和氟源气体，调节金属靶功率，沉积掺杂导电疏水层；
S6：根据所需薄膜的厚度，控制沉积时间，待沉积室内温度冷却至常温后取出样品。
7.根据权利要求6所述的一种具有疏水表面改性涂层的射频消融针的制备方法，其特征在于，所述步骤S1中，清洗是将针尖端在丙酮和去离子水中超声清洗。
8.根据权利要求6所述的一种具有疏水表面改性涂层的射频消融针的制备方法，其特征在于，所述步骤S3中，条件为在1.0Pa的气压与-900V的偏压。
9.根据权利要求6所述的一种具有疏水表面改性涂层的射频消融针的制备方法，其特征在于，所述步骤S4中，参数为：沉积气压范围为0.1Pa至10Pa，偏置电压范围为-50V至-200V、沉积温度范围为25℃至500℃。
10.根据权利要求6所述的一种具有疏水表面改性涂层的射频消融针的制备方法，其特征在于，所述步骤S5中，碳源气体为甲烷、乙烷、乙烯、乙炔和苯中的任意一种或其任何组合；氟源气体为四氟甲烷、六氟乙烷、八氟丙烷、四氟乙烯和六氟丙烯中的任意一种或其任何组合。
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