CN106111987B - 一种合金粉末制备涂层导体用NiW合金基带坯锭的方法 - Google Patents
一种合金粉末制备涂层导体用NiW合金基带坯锭的方法 Download PDFInfo
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- 238000005275 alloying Methods 0.000 description 1
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- FFWQPZCNBYQCBT-UHFFFAOYSA-N barium;oxocopper Chemical compound [Ba].[Cu]=O FFWQPZCNBYQCBT-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种合金粉末制备涂层导体用NiW合金基带坯锭的方法属于高温超导涂层导体用基带技术领域。本发明得到了W元素分布均匀且晶粒尺寸细小的NiW合金坯锭，经热轧开坯，冷轧及两步再结晶热处理后得到了强立方织构NiW合金基带。与传统工艺相比，此方法制备的NiW合金坯锭组织性能良好的同时工艺步骤简单，在大规模产业化应用中节能效益明显；适用范围广，可用于单层或复合NiW合金基带的坯锭制备。
Description
技术领域
本发明涉及一种强立方织构NiW合金基带坯锭的制备方法，属于高温超导涂层导体用基带技术领域。
背景技术
以YBa2Cu3O7-δ(YBCO)为代表的稀土类钡铜氧化物，属于高温超导材料，具有高的不可逆场，低的交流损耗，大大提升了超导材料的应用温度与磁场，但YBCO超导性能表现出强烈的各向异性，且与铋系、铁基、MgB2等其他高温超导材料相比，其相干长度很小，临界电流密度强烈地依赖于晶界夹角。为了获得YBCO薄膜优良的超导电性与机械性能，作为涂层导体基底的NiW合金基带，承担着外延织构与承受一定应力应变两大功能。因此高立方织构度、高强度NiW合金基带的制备是压延辅助双轴织构基板法(RABiTS)制备钇系高温超导材料的关键技术。
金属材料组织与织构的发展具有很强的“遗传性”，良好的坯锭基础是NiW合金基带后续大形变冷轧及再结晶过程的重要保障。涂层导体用NiW合金基带强立方织构的形成建立在初始坯锭中W元素的均匀分布与晶粒尺寸的控制上：W元素的偏聚使坯锭局部层错能迅速降低，导致应力集中形变不均匀，这对后续的铜型形变组织与强立方再结晶组织的形成来说是致命的打击；另一方面细化晶粒对立方织构形成的积极意义已在各文献中多次体现，相同的形变与再结晶条件下，晶粒尺寸小的坯锭形变过程更多的以位错滑移方式进行，形变更均匀。
目前NiW合金基带坯锭的制备主要分熔炼法与粉末冶金法两大方向，德国Dresden实验室采用熔炼法制备Ni9.3W、Ni9.5W合金基带，坯锭均匀化与晶粒细化采用了热锻、热轧、均匀化热处理及初始再结晶热处理四大步骤，工艺路线长，坯锭稳定性差。
2007年美国休斯顿大学提出粉末冷等静压烧结的方式，制备Ni9W合金基带；2008年赵跃采用放电等离子烧结，经坯锭均匀化热处理制备Ni9.3W合金基带；2010年邱火勤等人设计热等静压法(专利号：ZL201010167063.8)制备NiW合金复合基带。以上提及的粉末冶金法制备NiW合金基带均采用单质Ni粉单质W粉混合粉末球磨后置于石墨模具中进行烧结，Ni与W在高温高压过程中合金化形成NiW合金固溶体。此方法W难以在短时间内充分扩散均匀，研究人员常常采用1200℃、24h高温长时间均匀化热处理处理坯锭，但在保证W扩散均匀的同时晶粒尺寸不可避免地长大至80～100μm，因此，如何兼顾NiW合金坯锭W元素的均匀分布与细小晶粒尺寸的控制是NiW合金基带研究亟待解决的难题。
发明内容
本发明的目的是提出一种合金粉末制备涂层导体用NiW合金基带坯锭的方法，可以有效地避免传统粉末冶金法制备NiW合金坯锭W元素分布不均匀及均匀化热处理后晶粒尺寸过大的问题，促进了NiW合金基带轧制过程铜型形变织构及再结晶过程强立方织构的形成。
所选NiW合金粉末采用氩气雾化法生产，并在坯锭制备前进行球磨预处理。球磨预处理细化合金粉末颗粒的同时压实原始粉末中存在的空心粉，防止坯锭中引入封闭式气孔、杂质。
一种球磨合金粉末制备涂层导体用NiW合金基带的方法包括以下步骤：
(1)NiW合金粉末预处理
选取粒度为30～35μm、W原子百分含量为5～12的NiW合金粉末，置于高能球磨机中球磨得到粒度在10～15μm的合金粉末。球磨采用15mm、10mm、5mm三种直径的玛瑙球，球磨级配为大中小球质量比为1:4:3，球粉质量比为6:1；球磨过程在保护性气氛下进行，球磨转速为150～200rpm/min，球磨时间共7h。
(2)NiW合金粉末替代单质混合粉末放电等离子烧结
将步骤(1)得到的合金粉末置于石墨模具中，通过放电等离子烧结成型得到NiW合金坯锭。其中放电等离子烧结在真空条件下加压烧结，烧结压强为30MPa；烧结温度控制在850～880℃，升温速度为100℃/min，保温5min后随炉冷却。
(3)形变
将步骤(2)得到的NiW合金坯锭进行热轧开坯轧至8mm，轧制温度为900～1100℃，每道次轧制压下量与轧前厚度之比为20～30％；冷轧轧至0.08mm，每道次轧制压下量与轧前厚度之比5％；冷轧过程加入轧制中间热处理若干次(0-3次,即也可不加轧制中间热处理)来缓解大变形量轧制造成的加工硬化，轧制中间热处理温度为550℃，保温时间为60～120min。
(4)再结晶
将轧制好的NiW合金带材经两步再结晶热处理得到强立方织构NiW合金基带。第一步再结晶热处理温度为700～750℃保温60min，第二步再结晶热处理温度为1050～1250℃保温120min。
以上热处理均在H2体积分数为4％的Ar/H2混合气氛中进行，升温速度5℃/min，随炉冷却。
本发明设计的NiW合金粉末制备涂层导体用NiW合金基带坯锭的方法，得到了W元素分布均匀且晶粒尺寸细小的NiW合金坯锭，经热轧开坯，冷轧及两步再结晶热处理后得到了强立方织构NiW合金基带。与传统工艺相比，此方法制备的NiW合金坯锭组织性能良好的同时工艺步骤简单，在大规模产业化应用中节能效益明显；适用范围广，可用于单层(见实施例1与2)复合(见实施例3))NiW合金基带的坯锭制备。
附图说明
图1、实施例1中Ni8W轧制至0.08mm后形变组织(111)极图
图2、实施例1中Ni8W再结晶热处理后立方织构含量EBSD图
图3、实施例2中Ni5W轧制至0.08mm后形变组织(111)极图
图4、实施例2中Ni5W再结晶热处理后立方织构含量EBSD图
图5、实施例3中Ni8W/Ni12W/Ni8W轧制至0.08mm后形变组织(111)极图
图6、实施例3中Ni8W/Ni12W/Ni8W再结晶热处理后立方织构含量EBSD图
具体实施方式
下面结合实施例对本发明做进一步的说明，但本发明并不仅限于以下实施例。
实例1
选取粒度为30～35μm、W原子百分含量为8的NiW合金粉末，称量20g置于高能球磨机中球磨粒度在10～15μm的合金粉末。球磨采用玛瑙球，球磨级配为大中小球质量比为1:4:3，球粉质量比为6:1。球磨过程在H2体积分数为4％的Ar/H2混合气氛下进行，球磨机转速为200rpm/min，球磨时间共7h。球磨两次共得到40g Ni8W合金粉末。将所得合金粉末称量36.24g置于石墨模具中，通过放电等离子烧结成型，得到长宽高为20*15*13mm的Ni8W合金坯锭。放电等离子烧结在真空条件下加压烧结,烧结压强为30MPa，烧结温度控制在850～880℃，升温速度100℃/min，保温5min后随炉冷却。然后将此Ni8W合金坯锭磨抛至12mm后进行热轧开坯轧至8mm，轧制温度为1100℃，每道次轧制压下量与轧前厚度之比为20～30％。热轧后的合金基带去除表面氧化皮后冷轧轧至0.08mm，每道次轧制压下量与轧前厚度之比为5％。冷轧过程加入3次550℃保温120min的轧制中间热处理：第一次轧制中间热处理在轧至3mm时进行，第二次轧制中间热处理在轧至1mm时进行，第三次轧制中间热处理在轧至0.4mm时进行。轧制中间热处理在H2体积分数为4％的Ar/H2混合气氛中进行，升温速度5℃/min，随炉冷却。最后将轧制好的Ni8W合金带材经两步再结晶热处理得到得到立方织构含量(取向差10°以内)达96.5％的Ni8W基带。两步再结晶热处理在H2体积分数为4％的Ar/H2混合气氛中进行，第一步再结晶热处理温度为750℃保温60min，第二步再结晶热处理温度为1200℃保温120min，升温速度5℃/min随炉冷却。
实例2
选取粒度为30～35μm、W原子百分含量为5的NiW合金粉末，称量20g置于高能球磨机中球磨粒度在10～15μm的合金粉末。球磨采用玛瑙球，球磨级配为大中小球质量比为1:4:3，球粉质量比为6:1。球磨过程在H2体积分数为4％的Ar/H2混合气氛下进行，球磨机转速为200rpm/min，球磨时间共7h。球磨两次共得到40g Ni5W合金粉末。将所得合金粉末称量34.71g置于石墨模具中，通过放电等离子烧结成型，得到长宽高为20*15*12.8mm的Ni5W合金坯锭。放电等离子烧结在真空条件下加压烧结,烧结压强为30MPa，烧结温度控制在850～880℃，升温速度100℃/min，保温5min后随炉冷却。然后将此Ni5W合金坯锭磨抛至12mm后进行热轧开坯轧至8mm，轧制温度为900℃，每道次轧制压下量与轧前厚度之比为20～30％。热轧后的合金基带去除表面氧化皮后冷轧轧至0.08mm，每道次轧制压下量与轧前厚度之比为5％。最后将轧制好的Ni5W合金带材经两步再结晶热处理得到得到立方织构含量(取向差10°以内)达99％的Ni5W基带。两步再结晶热处理在H2体积分数为4％的Ar/H2混合气氛中进行，第一步再结晶热处理温度为700℃保温60min，第二步再结晶热处理温度为1200℃保温120min，升温速度5℃/min，随炉冷却。
实例3
选取粒度为30～35μm、W原子百分含量为8的NiW合金粉末,称量20g置于高能球磨机中球磨得到粒度在10～15μm的合金粉末。球磨采用玛瑙球，球磨级配为大中小球质量比为1:4:3，球粉质量比为6:1。球磨过程在H2体积分数为4％的Ar/H2混合气氛下进行，球磨机转速为200rpm/min，球磨时间共7h。球磨两次共得到40g Ni8W合金粉末。采用同样的方法球磨一次得到20g Ni12W合金粉末。分别称量Ni8W合金粉末12.08g、Ni12W合金粉末12.74g与Ni8W合金粉末12.08g逐层置于石墨模具中，通过放电等离子烧结成型，得到长宽高为20*15*13mm的Ni8W/Ni12W/Ni8W复合坯锭。放电等离子烧结在真空条件下加压烧结,烧结压强为30MPa，烧结温度控制在850～880℃，升温速度为100℃/min，保温5min后随炉冷却。然后将此Ni8W/Ni12W/Ni8W复合坯锭磨抛至12mm后进行热轧开坯轧至8mm，轧制温度为1100℃，每道次轧制压下量与轧前厚度之比为20～30％。热轧后的合金基带去除表面氧化皮后冷轧轧至0.08mm，每道次轧制压下量与轧前厚度之比为5％。冷轧过程加入3次550℃保温120min的轧制中间热处理：第一次轧制中间热处理在轧至3mm时进行，第二次轧制中间热处理在轧至1mm时进行，第三次轧制中间热处理在轧至0.4mm时进行。轧制中间热处理在H2体积分数为4％的Ar/H2混合气氛中进行，升温速度5℃/min，随炉冷却。最后将轧制好的Ni8W/Ni12W/Ni8W复合带材经两步再结晶热处理得到得到立方织构含量(取向差10°以内)达96％的Ni8W/Ni12W/Ni8W复合基带。两步再结晶热处理在H2体积分数为4％的Ar/H2混合气氛中进行，第一步再结晶热处理温度为750℃保温60min，第二步再结晶热处理温度为1250℃保温120min，升温速度5℃/min，随炉冷却。
Claims (2)
1.一种合金粉末制备涂层导体用NiW合金基带坯锭的方法，其特征在于，包括以下步骤：
(1)NiW合金粉末预处理
选取粒度为30～35μm、W原子百分含量为5～12的NiW合金粉末，置于高能球磨机中球磨得到粒度在10～15μm的合金粉末；球磨采用15mm、10mm、5mm三种直径的玛瑙球，球磨级配为大、中、小球质量比为1:4:3，球粉质量比为6:1；球磨过程在保护性气氛下进行，球磨转速为150～200rpm/min，球磨时间共7h；
(2)NiW合金粉末替代单质混合粉末放电等离子烧结
将步骤(1)得到的合金粉末置于石墨模具中，通过放电等离子烧结成型得到NiW合金坯锭；其中放电等离子烧结在真空条件下加压烧结，烧结压强为30MPa，烧结温度控制在850～880℃，升温速度为100℃/min，保温5min后随炉冷却；
(3)形变
将步骤(2)得到的NiW合金坯锭进行热轧开坯轧至8mm，轧制温度为900～1100℃，每道次轧制压下量与轧前厚度之比为20～30％；冷轧轧至0.08mm，每道次轧制压下量与轧前厚度之比5％；
(4)再结晶
将轧制好的NiW合金带材经两步再结晶热处理得到NiW合金基带；第一步再结晶热处理温度为700～750℃保温60min，第二步再结晶热处理温度为1050～1250℃保温120min；
以上热处理均在H2体积分数为4％的Ar/H2混合气氛中进行，升温速度5℃/min，随炉冷却。
2.根据权利要求1所述的方法，其特征在于，包括以下步骤：
冷轧过程加入轧制中间热处理1-3次，每次轧制中间热处理温度为550℃，保温时间为60～120min。
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