CN106222610B - 一种纳米复合硬质涂层及其制备方法 - Google Patents
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Abstract
本发明公开了一种纳米复合硬质涂层及其制备方法,是采用电弧离子镀和磁控溅射技术复合制备,通过周期性调节工艺参数,使电弧离子镀层即高应力层和磁控溅射层即低应力层分别交替循环沉积,从而有效地调整硬质涂层内的残余应力,获得纳米复合硬质涂层。本发明结合电弧离子镀技术离化率、入射粒子能量高和磁控溅射技术膜层均匀、表面平整等优点,同时考虑到材料热膨胀系数的差异,在金属基体表面镀一层过渡层,再复合制备多层纳米复合硬质涂层,通过调节涂层内的残余应力分布,在保持涂层高硬度及耐磨性能的前提下,可以进一步提高其膜基结合力。
Description
技术领域
本发明涉及表面处理技术领域,特别涉及一种纳米复合硬质涂层及其制备方法。
背景技术
电弧离子镀(AIP)和磁控溅射技术(MS)被广泛应用于制备涂层刀具。电弧离子镀技术具有离子能量高、离化率高、膜层致密和附着力强等优点,但电弧离子镀制备的薄膜容易含有显微喷溅颗粒,影响表面的粗糙度,破坏膜的连续性;而磁控溅射沉积技术制备的薄膜表面平整、致密,无明显的孔洞和电弧沉积时的大颗粒。此外,涂层残余应力的大小及其分布情况会直接影响膜基结合强度与涂层的使用寿命,甚至在残余应力过大时还将直接导致涂层的防护作用失效。电弧离子镀制备的涂层内一般都存在平均值高达数兆帕(MPa)甚至十几GPa的残余压应力,且应力沿层深分布极其不均匀;而磁控溅射镀膜制备的涂层内应力较小或一般为拉应力。因此,采用电弧离子镀(AIP)与磁控溅射(MS)复合制备多层纳米复合硬质涂层,不仅可以有效改善电弧离子镀技术制备的薄膜表面质量,还能提高膜层的硬度、韧性及结合力等综合力学性能,是目前提高硬质薄膜性能的重要发展方向之一。
发明内容
本发明的目的在于克服现有技术中存在的缺点,提供一种硬度高、耐磨性能好、膜基结合力强的纳米复合硬质涂层。
本发明的另一目的在于提供一种上述纳米复合硬质涂层的制备方法,是采用电弧离子镀(AIP)和磁控溅射(MS)技术复合制备。
本发明的目的通过下述技术方案实现:
一种纳米复合硬质涂层的制备方法,是采用电弧离子镀和磁控溅射技术复合制备,包括下述步骤:
(1)金属基体前处理工艺:金属基体先后经过酒精、金属洗涤剂、去离子水超声波清洗5~10min,然后用干燥洁净压缩空气吹干装入真空室内,预抽本底真空至3.0~5.0×10-3Pa;
(2)镀膜前预热至100~300℃,通入40~80sccm Ar气,升压至0.3~0.5Pa,基体加占空比30%~40%和600~800V的脉冲偏压,然后开启电弧靶,调节靶电流50~70A,进行弧光清洗5~10min,清洗基体和靶材表面的杂质和氧化物;
(3)保持其他参数不变,降低基体偏压至50~200V,沉积温度100~300℃,沉积2~4min,过渡层厚度为90~180nm;
(4)调节Ar和N2气流量阀,同时通入0~5sccm Ar和40~80sccm N2,工作气压升至0.5~1.0Pa,沉积温度100~300℃,沉积10~14min,电弧离子镀(AIP)层厚度为450~630nm;
(5)关闭电弧靶,调节Ar和N2气流量阀,同时通入20~30sccm Ar和1~5sccm N2,调节工作气压至0.3~0.5Pa,开启磁控靶,调节靶源功率100~300W,沉积温度100~300℃,沉积24~60min,磁控溅射(MS)层厚度大约180~450nm;
(6)通过周期性调节工艺参数,使电弧离子镀(AIP)层即高应力层和磁控溅射(MS)层即低应力层分别交替循环沉积,从而有效地调整硬质涂层内的残余应力,获得纳米复合硬质涂层。
一种纳米复合硬质涂层,是采用上述方法制备得到,高应力层(AIP)和低应力层(MS)交替循环沉积,且每一层厚度为100~500nm,总厚度为1~3μm。
本发明与现有技术相比具有如下优点和效果:
(1)本发明结合电弧离子镀(AIP)技术离化率、入射粒子能量高和磁控溅射(MS)技术膜层均匀、表面平整等优点,同时考虑到材料热膨胀系数的差异,在金属基体表面镀一层过渡层,再复合制备多层纳米复合硬质涂层,通过调节涂层内的残余应力分布,在保持涂层高硬度及耐磨性能的前提下,可以进一步提高其膜基结合力。
(2)本发明的制备工艺简单,操作方便。
附图说明
图1为本多层纳米复合硬质涂层的结构示意图。
其中,0—过渡层(增加结合力),
1—AIP层(高应力层),
2—MS层(低应力层)。
具体实施方式
下面结合实施例对本发明做进一步详细的描述,但本发明的实施方式不限于此。
实施例1
本实施例采用电弧与磁控复合制备多层纳米复合硬质涂层,同时考虑到材料热膨胀系数的差异(不锈钢:18.6×10-6,Ti涂层:10.8×10-6,TiN涂层:9.4×10-6),在316L不锈钢表面镀一层过渡层Ti(增加涂层的结合力),再交替循环沉积TiN多层纳米复合硬质涂层,如图1所示,过渡层Ti厚度约90nm,交替层TiN每一层厚度约450nm,总厚度约2.34μm。
(1)基体前处理工艺:不锈钢样品先后经过酒精、金属洗涤剂、去离子水超声波清洗5min,然后用干燥洁净压缩空气吹干装入真空室内,预抽本底真空至5.0×10-3Pa;
(2)镀膜前预热至100℃,通入80sccm Ar气,升压至0.5Pa,基体加占空比40%和800V的脉冲偏压,开启电弧纯Ti靶(99.99%),调节靶电流60A,进行弧光清洗5min,清洗基体和靶材表面的杂质和氧化物;
(3)保持其他参数不变,降低基体偏压至150V,沉积温度100℃,沉积2min,Ti过渡层厚度大约90nm;
(4)调节Ar和N2气流量阀,同时通入5sccm Ar和75sccm N2,工作气压升至1.0Pa,沉积温度100℃,沉积10min,TiN(AIP)层厚度约450nm;
(5)关闭电弧靶,调节Ar和N2气流量阀,同时通入30sccm Ar和0.4sccm N2,调节工作气压至0.4Pa,开启磁控纯Ti靶(99.99%),调节靶源功率180W,沉积温度100℃,沉积60min,TiN(MS)层厚度约450nm;
(6)通过周期性调节工艺参数,使涂层的高应力层和低应力层分别交替循环沉积3次和2次,即获得TiN多层纳米复合涂层的制备。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (2)
1.一种纳米复合硬质涂层的制备方法,其特征在于:是采用电弧离子镀和磁控溅射技术复合制备,包括下述步骤:
(1)金属基体前处理工艺:金属基体先后经过酒精、金属洗涤剂、去离子水超声波清洗5~10min,然后用干燥洁净压缩空气吹干装入真空室内,预抽本底真空至3.0~5.0×10-3Pa;
(2)镀膜前预热至100~300℃,通入40~80sccm Ar气,升压至0.3~0.5Pa,基体加占空比30%~40%和600~800V的脉冲偏压,然后开启电弧靶,调节靶电流50~70A,进行弧光清洗5~10min,清洗基体和靶材表面的杂质和氧化物;
(3)保持其他参数不变,降低基体偏压至50~200V,沉积温度100~300℃,沉积2~4min,过渡层厚度为90~180nm,过渡层的材质为Ti;
(4)调节Ar和N2气流量阀,同时通入0~5sccm Ar和40~80sccm N2,工作气压升至0.5~1.0Pa,沉积温度100~300℃,沉积10~14min,电弧离子镀层厚度为450~630nm;
(5)关闭电弧靶,调节Ar和N2气流量阀,同时通入20~30sccm Ar和1~5sccm N2,调节工作气压至0.3~0.5Pa,开启磁控靶,调节靶源功率100~300W,沉积温度100~300℃,沉积24~60min,磁控溅射层厚度大约180~450nm;
(6)通过周期性调节工艺参数,使电弧离子镀层即高应力层和磁控溅射层即低应力层分别交替循环沉积,高应力层和低应力层的材质为TiN,从而有效地调整硬质涂层内的残余应力,获得纳米复合硬质涂层。
2.一种纳米复合硬质涂层,其特征在于:是采用权利要求1所述的纳米复合硬质涂层的制备方法制备得到,高应力层和低应力层交替循环沉积,且每一层厚度为100~500nm,总厚度为1~3μm。
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