CN108588588A - 金属/非晶合金扩散偶的制备方法 - Google Patents
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Abstract
金属/非晶合金扩散偶的制备方法,包括块体非晶合金的制备,将步骤一中的得到的棒材切割成试样,在丙酮中进行超声波清洗和脱脂;将样品安放在磁控溅射室内的阴极靶位上开启磁控溅射设备中的离子清洗;镀膜后的样品密封在真空玻璃管内,最后通过扩散退火热处理之后,试样快速冷却至室温,得到金属/非晶合金扩散偶;本发明具有能够使得非晶基体组织基本无变化,仍然保持非晶态的优点。
Description
技术领域
本发明涉及材料焊接领域,特别涉及金属/非晶合金扩散偶的制备方法。
背景技术
块体金属玻璃具有非常好的弹性极限和高的屈服强度,高硬度和强度,非常好的耐腐蚀性能,低的热导,能直接加工成型等优良特性,适合于制造军事产品,并有望在环保型动能穿甲弹,高性能复合装甲,高耐磨表面硬化和轻量化部件,抗腐蚀部件和电子器件保护套,轻量化和高强度结构部件等军事部件中进行应用。尽管非晶合金具有较好的应用前景,但是由于非晶合金本身尺寸效应以及室温塑性差等方面的限制,阻碍了非晶合金作为工程结构材料等方面的应用。为了解决非晶合金尺寸效应及室温塑性差的限制,拓宽非晶合金工程化应用,近几年一些新技术的发现,如:爆炸焊接、摩擦焊、电子束焊、共压及共挤等方法的引入成功实现了非晶合金/非晶合金,非晶合金/金属的连接,并具有良好的力学性能,进一步推进了非晶合金在工程方面的应用。比如说通过电子束方法将Zr41Ti14Cu12Ni10Be23非晶合金与纯Zr(Y.Kawamura,T.Shoji,Y.Ohno.Welding of bulkmetallic glasses.Journal of Non-Crystalline Solids.2003,317:152-157),Zr41Ti14Cu12Ni10Be23非晶合金与纯Ti(S.Kagao,Y.Kawamura,Y.Ohno.Electron-beamwelding of Zr-based bulk metallic glasses.Materials Science and Engineering:A.2004,375-377:312-316)进行焊接,两个界面呈现的结果差异很大,前者界面可以达到原子级别的冶金结合,并具有较好的力学性能(拉伸强度与纯Zr的相当);而后者在界面处形成了脆性相,导致无法施展力学性能测试。此后,Kim还发现通过此方法获得的Zr41Ti14Cu12Ni10Be23非晶合金/Ni界面状态与电子束辐照位置有关。
原子在非晶合金中的扩散距离较短(仅为20nm-100nm)并且扩散系数很低,很难采用传统的电子探针(EPMA)以及能谱(EDS)等方法来研究。此外,非晶合金的热稳定性对成分较为敏感,当焊接界面存在氧原子夹杂之后,将使界面处的热稳定性降低,形成纳米晶。同样,当界面有大量氧化膜存在时,也将进一步阻碍基体内原子的相互扩散,降低扩散系数,最终导致连接失败。因此,采用传统的焊接法制备金属/非晶合金扩散偶是不合理的。
发明内容
为了克服上述现有技术的不足,本发明提供了金属/非晶合金扩散偶的制备方法,能够清除非晶合金表面的杂质原子,进而使金属原子与非晶合金达到原子级别的结合,非晶基体组织基本无变化,仍然保持非晶态。
为了达到上述目的,本发明采用的技术方案为:
金属/非晶合金扩散偶的制备方法,其步骤为:
步骤一:块体非晶合金的制备
将母合金放入吸铸坩埚,用氩气洗炉,再将炉腔真空抽至3.0×10-3Pa,在氩气保护下采用感应熔炼的方法将母合金熔化并将熔体吸铸到模具中,获得棒材;
步骤二:预处理
将步骤一中的得到的棒材切割成试样,将试样用于镀膜的圆截面用砂纸依次打磨并且机械抛光,确保截面没有划痕后,在丙酮中进行超声波清洗和脱脂3~5min,放置于磁控溅射镀膜设备的真空炉中,进行抽真空,得到靶材;
步骤三:将步骤二中得到的靶材安放在磁控溅射室内的阴极靶位上,用机械泵及分子泵将溅射室抽到真空度为6×10-4Pa,开启磁控溅射设备中的离子清洗,将清洗好的靶材定在衬底托盘上放入过渡舱室,抽真空为3.4×10-4Pa,反溅射清洗样品3min;然后再送至溅射室,通入氩气后采用射频磁控溅射清洗靶材5min,然后对非晶态合金表面进行镀膜,得到镀膜样品;
步骤四:镀膜后的样品密封在真空玻璃管内,加热到非晶合金玻璃态/过冷液相区的温度值时进行保温,最后通过扩散退火热处理之后,试样快速冷却至室温,得到金属/非晶合金扩散偶。
所述的步骤一的棒材形状为Φ5×50mm。
所述的步骤二的试样的形状为Φ5×2mm。
所述的镀膜厚度为100nm。
所述的真空玻璃管内的真空度高于10-4Pa。
本发明的有益效果;
本发明采用磁控溅射设备中的离子清洗,清除非晶合金表面的杂质原子,进而使金属原子与非晶合金达到原子级别的结合,非晶基体组织基本无变化,仍然保持非晶态,然后封装热处理,进而获得理想状态的扩散偶。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1
Ni/Zr48Cu36Ag8Al8非晶合金扩散偶的制备方法,其步骤为:
步骤一:Zr48Cu36Ag8Al8非晶合金制备
将母合金放入吸铸坩埚,用氩气洗炉1次,再将炉腔真空抽至3.0×10-3Pa,在氩气保护下采用感应熔炼的方法将母合金熔化并将熔体吸铸到模具中,获得Φ5×50mm棒材;
步骤二:预处理
将步骤一中的得到的Φ5×50mm棒材切割成Φ5×2mm的试样,切割过程中要加大冷却水的流量以减小此过程对非晶结构的影响防止晶化,将试样用于镀膜的圆截面用砂纸依次打磨并且机械抛光,确保截面没有划痕后,在丙酮中进行超声波清洗和脱脂3~5min,共两次后,放置于磁控溅射镀膜设备的真空炉中,进行抽真空,得到靶材;
步骤三:将步骤二中得到的靶材安放在磁控溅射室内的阴极靶位上,用机械泵及分子泵将溅射室抽到真空度为6×10-4Pa,开启磁控溅射设备中的离子清洗,将清洗好的靶材定在衬底托盘上放入过渡舱室,并调整相应位置,抽真空为3.4×10-4Pa,反溅射清洗样品3min;然后再送至溅射室,通入氩气后采用射频磁控溅射清洗靶材5min,然后对非晶态Zr48Cu36Ag8Al8合金表面进行镀Ni,薄膜厚度约为100nm,得到镀膜样品;
步骤四:镀膜后的样品密封在真空玻璃管内,真空度高于10-4Pa,加热到非晶合金玻璃态/过冷液相区的温度值时进行保温,最后通过扩散退火热处理之后,试样快速冷却至室温,得到金属/非晶合金扩散偶。
实施例2
Ni/Zr41.2Ti13.8Ni10Cu12.5Be22.5非晶合金扩散偶的制备方法,其步骤为:
步骤一:Zr41.2Ti13.8Ni10Cu12.5Be22.5非晶合金制备
将母合金放入吸铸坩埚,用氩气洗炉1次,再将将炉腔真空抽至3.0×10-3Pa,在氩气保护下采用感应熔炼的方法将母合金熔化并将熔体吸铸到模具中,获得Φ9×50mm棒材;
步骤二:预处理
将步骤一中的得到Φ9×50mm棒材切割成Φ9×2mm的试样,将试样用于镀膜的圆截面用砂纸依次打磨并且机械抛光,确保截面没有划痕后,在丙酮中进行超声波清洗和脱脂3~5min共两次,放置于磁控溅射镀膜设备的真空炉中,进行抽真空,靶材;
步骤三:将步骤二中得到的靶材安放在磁控溅射室内的阴极靶位上,用机械泵及分子泵将溅射室抽到真空度为6×10-4Pa,开启磁控溅射设备中的离子清洗,将清洗好的靶材定在衬底托盘上放入过渡舱室,并调整相应位置,抽真空为3.4×10-4Pa,反溅射清洗样品3min;然后再送至溅射室,通入氩气后采用射频磁控溅射清洗靶材5min,然后对非晶态Zr41.2Ti13.8Ni10Cu12.5Be22.5合金表面进行镀Ni,薄膜厚度约为100nm,得到镀膜样品;
步骤四:镀膜后的样品密封在真空玻璃管内,真空度高于10-4Pa,加热到非晶合金玻璃态/过冷液相区的温度值时进行保温,最后通过扩散退火热处理之后,试样快速冷却至室温,得到金属/非晶合金扩散偶。
Claims (5)
1.金属/非晶合金扩散偶的制备方法,其特征在于,其步骤为:
步骤一:块体非晶合金的制备
将母合金放入吸铸坩埚,用氩气洗炉,再将将炉腔真空抽至3.0×10-3Pa,在氩气保护下采用感应熔炼的方法将母合金熔化并将熔体吸铸到模具中,获得棒材;
步骤二:预处理
将步骤一中的得到的棒材切割成试样,将试样用于镀膜的圆截面用砂纸依次打磨并且机械抛光,确保截面没有划痕后,在丙酮中进行超声波清洗和脱脂3~5min,放置于磁控溅射镀膜设备的真空炉中,进行抽真空,得到靶材;
步骤三:将步骤二中得到的靶材安放在磁控溅射室内的阴极靶位上,用机械泵及分子泵将溅射室抽到真空度为6×10-4Pa,开启磁控溅射设备中的离子清洗,将清洗好的靶材定在衬底托盘上放入过渡舱室,抽真空为3.4×10-4Pa,反溅射清洗样品3min;然后再送至溅射室,通入氩气后采用射频磁控溅射清洗靶材5min,然后对非晶态合金表面进行镀膜,得到镀膜样品;
步骤四:镀膜后的样品密封在真空玻璃管内,加热到非晶合金玻璃态/过冷液相区的温度值时进行保温,最后通过扩散退火热处理之后,试样快速冷却至室温,得到金属/非晶合金扩散偶。
2.根据权利要求1所述的金属/非晶合金扩散偶的制备方法,其特征在于,所述的步骤一的棒材形状为Φ5×50mm。
3.根据权利要求1所述的金属/非晶合金扩散偶的制备方法,其特征在于,所述的步骤二的试样的形状为Φ5×2mm。
4.根据权利要求1所述的金属/非晶合金扩散偶的制备方法,其特征在于,所述的镀膜厚度为100nm。
5.根据权利要求1所述的金属/非晶合金扩散偶的制备方法,其特征在于,所述的真空玻璃管内的真空度高于10-4Pa。
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