CN113355630B - 铝合金表面硬度涂层的制备方法 - Google Patents

铝合金表面硬度涂层的制备方法 Download PDF

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CN113355630B
CN113355630B CN202110910984.7A CN202110910984A CN113355630B CN 113355630 B CN113355630 B CN 113355630B CN 202110910984 A CN202110910984 A CN 202110910984A CN 113355630 B CN113355630 B CN 113355630B
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杨红娜
蔡风园
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Beijing Aerospace Hexing Technology Co Ltd
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Abstract

本申请涉及物理气相沉积成膜方法，具体为铝合金表面硬度涂层的制备方法。本申请在铝合金表面通过过渡层结构及交替复合膜层的制备，得到较高硬度的涂层，涂层与基体间结合性能也得到了改善。ZrAlTiN/AlTiN多层复合涂层结构设计，能够改善层间残余应力、硬度和断裂韧性之间的平衡，防止裂纹扩散。

Description

铝合金表面硬度涂层的制备方法
技术领域
本申请涉及物理气相沉积成膜方法，具体为铝合金表面硬度涂层的制备方法。
背景技术
铝合金，其具有比强度高、加工和成形性好、成本低以及可维修性好等一系列优点，被广泛应用于航空航天领域。火箭导弹等航天器的筒段、燃料箱、构件、骨架、外罩等结构部件和飞机的机翼、大梁等都大量使用了铝合金材料。铝合金材料较其他金属，比重量更低，有利于飞行器的减重，提高飞行经济性，增大航程。但是现有铝合金材料存在硬度不足的问题，当表面存在划痕或受外力后出现凹凸变形后，会影响飞行器的整体气动外形和结构强度。
物理气相沉积是新兴的一种表面涂层制备方法，可分为蒸镀、磁控溅射、离子镀等，其在高硬度膜层制备上的应用已经广泛展开，但是膜层与基体间的性质差异会导致膜基间存在开裂脱落的趋势，此外由于高硬度涂层自身内应力较高也存在产生裂纹的风险。
发明内容
本申请在铝合金表面通过过渡层及交替复合膜层的制备，得到较高硬度的涂层，涂层与基体间结合性能也得到了改善。具体的制备方法包括以下步骤：
基底预轰击：将处理腔加热至350～450℃，对腔体抽真空，使气压降至1×10-2-5×10-2Pa；打开基体偏压至-800～-1000V，然后通入25～30sccm的氩气，对铝合金基体表面进行Ar+轰击，在清洁基体表面的同时，使得铝合金基底表面暴露于腔室中，提高表面活性，便于后续反应能够进行。
制备得到氧化铝层：通入100～150sccm的O2，调整气压至0 .6～1 .5Pa，偏压为-60～-150V，使得被Ar+轰击后的铝合金表面氧化，得到氧化铝层。得到的氧化铝层起到过渡的作用，使得基体与后续物理气相沉积法制备得到的涂层之间结合力提高。
制备得到AlN过渡层：将基体偏压调至-80～-180V，通入250～400sccm的N2，点燃Al靶，调节气压至1×10-3-5×10-3Pa，腔室温度仍维持在350～450℃，脉冲电弧电源输出平均电流60～90A，频率：5～200Hz，占空比30％，沉积0.3微米厚度AlN过渡层，避免后续涂层与基体之间亲和性差异较大、层间应力过高。
制备ZrAlTiN/AlTiN交替复合层：基体置于腔室中心位置，ZrAlTi靶与AlTi靶分别置于基体两侧，基体在支架的带动下旋转，旋转速度1.5r/min，交替面向ZrAlTi靶与AlTi靶，最终溅射得到ZrAlTiN/AlTiN交替多层结构，通入25～40sccm的N2，调节气压至1×10-3-5×10-3Pa，真空腔室温度350～450℃，偏压-150～-180V，ZrAlTi靶、AlTi靶脉冲电流分别为90A和40A，ZrAlTiN/AlTiN复合层中ZrAlTiN层与AlTiN层调制比为2:1，调制周期为30～35nm最终，打开真空室取出样品，冷却至室温。该交替复合层中形成ZrN、AlTiN等氮化物相，硬度较高，采用交替多层结构能够降低涂层的内应力，提高涂层韧性，降低层间开裂的趋势。
ZrAlTi靶成分为：Zr 81.7At%，Al 15.2At%，Ti 3.1At%；
AlTi靶成分为：Al 50At%，Ti 50At%。
本申请在铝合金表面通过过渡层结构及交替复合膜层的制备，得到较高硬度的涂层，涂层与基体间结合性能也得到了改善。ZrAlTiN/AlTiN多层复合涂层结构设计，能够改善层间残余应力、硬度和断裂韧性之间的平衡，防止裂纹扩散。
具体实施方式
实施例1
基底预轰击：将处理腔加热至400℃，对腔体抽真空，使气压降至3×10-2Pa；打开基体偏压至-900V，然后通入30sccm的氩气；
制备得到氧化铝层：通入100sccm的O2，调整气压至1Pa，偏压为-110V，使得被Ar+轰击后的铝合金表面氧化，得到氧化铝层；
制备得到AlN过渡层：将基体偏压调至-100V，通入350sccm的N2，点燃Al靶，调节气压至3×10-3Pa，腔室温度仍维持在400℃，脉冲电弧电源输出平均电流70A，频率：110Hz，占空比30％，沉积0.3微米厚度AlN过渡层，避免后续涂层与基体之间亲和性差异较大、层间应力过高。
制备ZrAlTiN/AlTiN交替复合层：基体置于腔室中心位置，ZrAlTi靶与AlTi靶分别置于基体两侧，基体在支架的带动下旋转，旋转速度1.5r/min，交替面向ZrAlTi靶与AlTi靶，最终溅射得到ZrAlTiN/AlTiN交替多层结构，通入30sccm的N2，调节气压至2×10-3Pa，真空腔室温度400℃，偏压-150V，ZrAlTi靶、AlTi靶脉冲电流分别为90A和40A，ZrAlTiN/AlTiN复合层中ZrAlTiN层与AlTiN层调制比为2:1，调制周期为30～35nm；ZrAlTi靶成分为：Zr81.7At%，Al 15.2At%，Ti 3.1At%；AlTi靶成分为：Al 50At%，Ti 50At%。交替复合层中形成ZrN、AlTiN等氮化物相，硬度较高，采用交替多层结构能够降低涂层的内应力，提高涂层韧性，降低层间开裂的趋势，划痕法检测结合力达到60N，硬度为32.1GPa。
实施例2
基底预轰击：将处理腔加热至420℃，对腔体抽真空，使气压降至4×10-2Pa；打开基体偏压至-850V，然后通入30sccm的氩气；
制备得到氧化铝层：通入150sccm的O2，调整气压至1.2Pa，偏压为-100V，使得被Ar+轰击后的铝合金表面氧化，得到氧化铝层；
制备得到AlN过渡层：将基体偏压调至-90V，通入400sccm的N2，点燃Al靶，调节气压至2×10-3Pa，腔室温度仍维持在400℃，脉冲电弧电源输出平均电流70A，频率：110Hz，占空比30％，沉积0.3微米厚度AlN过渡层，避免后续涂层与基体之间亲和性差异较大、层间应力过高。
制备ZrAlTiN/AlTiN交替复合层：基体置于腔室中心位置，ZrAlTi靶与AlTi靶分别置于基体两侧，基体在支架的带动下旋转，旋转速度1.5r/min，交替面向ZrAlTi靶与AlTi靶，最终溅射得到ZrAlTiN/AlTiN交替多层结构，通入40sccm的N2，调节气压至2×10-3Pa，真空腔室温度400℃，偏压-160V，ZrAlTi靶、AlTi靶脉冲电流分别为90A和40A，ZrAlTiN/AlTiN复合层中ZrAlTiN层与AlTiN层调制比为2:1，调制周期为30～35nm；ZrAlTi靶成分为：Zr81.7At%，Al 15.2At%，Ti 3.1At%；AlTi靶成分为：Al 50At%，Ti 50At%。交替复合层中形成ZrN、AlTiN等氮化物相，硬度较高，采用交替多层结构能够降低涂层的内应力，提高涂层韧性，降低层间开裂的趋势，划痕法检测结合力达到63N，硬度为31.4GPa。

Claims (2)

1.一种铝合金表面硬度涂层的制备方法，其特征在于，
制备得到氧化铝层：通入100～150sccm的O2，调整气压至0 .6～1 .5Pa，偏压为-60～-150V，使得被Ar+轰击后的铝合金表面氧化，得到氧化铝层；
制备得到AlN过渡层：将基体偏压调至-80～-180V，通入250～400sccm的N2，点燃Al靶，调节气压至1×10-3～5×10-3Pa，腔室温度仍维持在350～450℃，脉冲电弧电源输出平均电流60～90A，频率：5～200Hz，占空比30％；
制备ZrAlTiN/AlTiN交替复合层：通入25～40sccm的N2，调节气压至1×10-3～5×10- 3Pa，真空腔室温度350～450℃，偏压-150～-180V，ZrAlTi靶、AlTi靶脉冲电流分别为90A和40A，ZrAlTi靶成分为：Zr 81.7At%，Al 15.2At%，Ti 3.1At%；AlTi靶成分为：Al 50At%，Ti50At%，ZrAlTiN/AlTiN复合层中ZrAlTiN层与AlTiN层调制比为2:1，调制周期为30～35nm，制备ZrAlTiN/AlTiN交替复合层过程中基体置于腔室中心位置，ZrAlTi靶与AlTi靶分别置于基体两侧，基体在支架的带动下旋转，旋转速度1.5r/min，交替面向ZrAlTi靶与AlTi靶，溅射得到ZrAlTiN/AlTiN交替多层结构，最终，打开真空室取出样品，冷却至室温。
2.根据权利要求1所述的制备方法，其特征在于，还包括基底预轰击步骤，将处理腔加热至350～450℃，对腔体抽真空，使气压降至1×10-2～5×10-2Pa；打开基体偏压至-800～-1000V，然后通入25～30sccm的氩气，对铝合金基体表面进行Ar+轰击，在清洁基体表面的同时，使得铝合金基底表面暴露于腔室中，提高表面活性，便于后续反应能够进行。
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CN111304612B (zh) * 2020-03-30 2022-02-08 天津职业技术师范大学(中国职业培训指导教师进修中心) 具有高硬度和高抗氧化性能的CrAlN/AlN纳米多层涂层及其制备方法

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