CN109576644A - 一种制备涂层导体用高钨合金基带的方法 - Google Patents
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract
一种制备涂层导体用高钨合金基带的方法属于金属加工技术领域。清洗Ni5W(W元素的含量＝5at.％)合金基带后，采用物理或化学的方法在其外表面均匀涂覆厚度为100～200nm的纯钨层。将上述涂覆钨层的Ni5W合金基带在氩氢或氢气的保护气氛下进行扩散热处理，热处理温度为1100～1200℃，保温时间2～3h，随炉冷却，使镀层表面的钨原子以置换固溶体的方式大量扩散至芯层置换晶格中的镍原子，以提高具有立方织构的NiW合金基带的钨含量，以获得具有强立方织构的高钨复合基带。本发明使表层的W原子大量渗入芯层，提高整体钨含量，获得织构高钨合金基带。该方法操作简单，成本较低，可实现性强。
Description
技术领域
本发明涉及一种用于第二代高温超导YBCO(YBa2Cu3O7-u，钇钡铜氧)涂层导体的高钨含量(W元素的含量≥7at.％)NiW合金基带的制备方法，属于金属加工技术领域。
背景技术
YBCO高温超导材料作为超导材料中的核心之一，具有良好的应用发展前景以及现实可行的实现路径，对高性能涂层超导材料的研究具有巨大的社会效益，而作为外延生长YBCO的织构NiW合金基带是RABiTS技术路线研究的热点。NiW合金基带在超导带材的结构中位于整个结构的底层，其主要作用是外延生长过渡层和超导层，同时承受一定的应力应变。在NiW合金中，虽然低钨含量的NiW合金容易获得强立方织构，但其强度及磁性能依然不能满足涂层导体应用的广泛要求；而高钨含量的NiW合金能实现应用温度下(77K，液氮温区)低铁磁性甚至无磁性，同时也带来了另一个不可避免的难题，即W元素固溶含量的增加降低了NiW合金的层错能，使材料形变与再结晶过程不再容易获得强立方织构。因此如何在提高钨含量的同时又能获得强立方织构，成为高钨合金基带进一步发展的方向与目标。
制备复合基带是一种获得高强度低磁性的NiW合金基带的有效思路。目前为止，研究人员提出多种方法来制备RABiTS路线的复合基带，主要有套管法、共轧制法和粉末冶金法等，这些方法的主要思路是将易形成立方织构的低钨含量NiW合金放在外层，机械强度高、铁磁性低的高钨含量NiW合金放在内层，形成“三明治”结构，以便获得立方织构和机械性能、铁磁性相统一的NiW合金基带。其中套管法是最早提出制备复合基带技术路线之一，但该技术路线无论是在形变过程中，还是在再结晶过程中，都受内、外层材料性质严重影响，并且加工工艺比较复杂。共轧制法虽是一种可大规模生产复合基带的方法，但这种工艺对轧制设备要求较高，一般较难实现。而粉末冶金法制备出的复合基带不同W含量的层间结合力相对较弱造成轧制过程中复合坯锭容易产生开裂现象，以及W由高浓度区域向低浓度区域发生扩散影响低钨层强立方织构的形成。
第二代高温超导YBCO涂层导体对NiW合金基带的要求是具有一定长度、表面具有强立方织构，同时基带整体又拥有高机械强度和低铁磁性，上述方法都是采用的外低钨内高钨结构、先加工形变再进行热处理获得立方织构的技术路线来制备复合基带。如果采用先低钨获得强立方织构、再进行渗钨的操作来提高钨含量，将是一条全新的制备路线，可有效前述制备方法的弊端。
发明内容
本发明的目的是提出一种先利用低钨含量NiW合金基带获得强立方织构、再通过在基带表面制备纯钨镀层形成外高钨内低钨的结构，利用钨原子扩散来提升NiW合金基带的整体钨含量，进而获得涂层导体用高钨合金基带的方法，该方法可以有效地提高合金基带的钨含量，提升NiW合金基带整体的机械性能，降低铁磁性。
一种制备涂层导体用高钨合金基带的方法包括以下步骤：
(1)清洗Ni5W(W元素的含量＝5at.％)合金基带后，采用物理或化学的方法在其外表面均匀涂覆厚度为100～200nm的纯钨层。
(2)将上述涂覆钨层的Ni5W合金基带在氩氢或氢气的保护气氛下进行扩散热处理，热处理温度为1100～1200℃，保温时间2～3h，随炉冷却，使镀层表面的钨原子以置换固溶体的方式大量扩散至芯层置换晶格中的镍原子，以提高具有立方织构的NiW合金基带的钨含量，以获得具有强立方织构的高钨复合基带。
本发明设计的制备涂层导体用高钨合金基带的方法，与传统工艺相比，创新性地在具有强立方织构的低钨合金基带表面涂覆一定厚度的纯钨镀层，形成外高钨内低钨的结构；再整体进行扩散退火热处理，可有效减少镀层中的应力，提高金属基底与镀层间的结合力；而后利用表层与芯层的浓度差，进行扩散热处理，使表层的W原子大量渗入芯层，提高整体钨含量，获得织构高钨合金基带。该方法操作简单，成本较低，可实现性强，具有大规模实际应用的前景。
附图说明
图1、实施例1中合金基带在1100℃下保温3h后的(111)极图；
图2、实施例2中合金基带在1200℃下保温2h后的(111)极图；
具体实施方式
以下所述为本发明较佳的一些实施例，对本发明的内容进行进一步详细描述，但是本发明的保护范围不限于这些实施例，凡是未脱离本发明技术方案的专利的内容，依据实施例进行任何简单修改、等同替换等都属于本发明的保护范围。
实例1【磁控溅射方法】
磁控溅射技术是在真空中利用荷能粒子轰击靶表面，使被轰击出的粒子沉积在基片上的技术，其特点是成膜速率高，基片温度低，镀膜层致密、均匀、膜的粘附性好，可实现大面积镀膜，因此我们首先采用磁控溅射法在低钨合金基带表面溅镀纯钨层，再结合扩散热处理工艺，得到低磁性、高强度、强立方织构的复合合金基带。
以纯度为99.9％的高纯钨靶作为溅射靶材，将其安放在高真空磁控溅射系统的直流靶位上。其次对退火后的Ni5W基底先使用丙酮和无水乙醇分别超声清洗5min并快速吹干后，将基带转移至磁控溅射设备样品台中心部位，关闭磁控溅射进样室。然后进行抽真空，至背底真空度为8×10-4Pa时，打开气路，对反应室通入氩气，同时对样品台加热至350℃，调节样品台转速为15r/min，溅射功率为100W，溅射时长为40min，在基底表面溅镀均匀致密的纯钨镀层。最后在H2体积分数为4％的氩氢混合气氛下进行扩散热处理，随炉升温至1100℃，保温时间为3h，随炉冷却后，用XRD对其进行测试，结果如图1所示。
实例2【化学气相沉积方法】
化学气相沉积技术是在高温下，通过气态初始化合物之间的气相化学反应而形成固体物质沉积在基体上的工艺技术，其特点是沉积成膜装置简单，薄膜表面致密性、均匀性均较高，内部应力均匀，缺陷少。
首先将Ni5W基底使用丙酮和无水乙醇分别超声清洗5min并快速吹干，其次将Ni5W基带放置到化学气相沉积装置的恒温加热区并抽真空至1×10-4Pa后，打开气路，对其通入反应气，气体成分的体积百分比为WF：H2＝6：4，气流量控制在60sccm，在生长过程中保持流速稳定不变，同时对样品加热至600℃后，保温20min，在基底表面沉积均匀致密的纯钨层。最后在H2气氛下进行扩散热处理，随炉升温至1200℃，保温时间为2h，随炉冷却。用XRD对其进行测试，结果如图2所示。
Claims (3)
1.一种制备涂层导体用高钨合金基带的方法，其特征在于，包括以下步骤：
(1)清洗Ni5W合金基带后，即合金基带中W元素的含量＝5at.％；采用物理或化学的方法在其外表面均匀涂覆厚度为100～200nm的纯钨层；
(2)将上述涂覆钨层的Ni5W合金基带在氩氢混合气氛或氢气的保护气氛下进行扩散热处理，热处理温度为1100～1200℃，保温时间2～3h，随炉冷却，得到高钨合金基带。
2.根据权利要求1所述的方法，其特征在于：
对退火后的Ni5W基底先使用丙酮和无水乙醇分别超声清洗5min并吹干后，将基带转移至磁控溅射设备样品台中心部位，关闭磁控溅射进样室；然后进行抽真空，至背底气压为8×10-4Pa以下时，打开气路，对反应室通入氩气，同时对样品台加热至350℃，调节样品台转速为15r/min，以钨靶作为溅射靶材，溅射功率为100W，溅射时长为40min，在基底表面溅镀均匀致密的纯钨镀层；最后在H2体积分数为4％的氩氢混合气氛下进行扩散热处理，随炉升温至1100℃，保温时间为3h，随炉冷却。
3.根据权利要求1所述的方法，其特征在于：
首先将Ni5W基底使用丙酮和无水乙醇分别超声清洗5min并吹干，其次将Ni5W基带放置到化学气相沉积装置的恒温加热区并抽真空至气压为1×10-4Pa以下后，打开气路，对其通入反应气，反应气体成分的体积比为WF：H2＝6：4，气流量控制在60sccm，在生长过程中保持流速稳定不变，同时对样品加热至600℃后，保温20min，在基底表面沉积均匀致密的纯钨层；最后在H2气氛下进行扩散热处理，随炉升温至1200℃，保温时间为2h，随炉冷却。
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