CN102758182A - 铁基合金表面镀膜方法及由该方法其制得的镀膜件 - Google Patents

铁基合金表面镀膜方法及由该方法其制得的镀膜件 Download PDF

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CN102758182A
CN102758182A CN2011101063485A CN201110106348A CN102758182A CN 102758182 A CN102758182 A CN 102758182A CN 2011101063485 A CN2011101063485 A CN 2011101063485A CN 201110106348 A CN201110106348 A CN 201110106348A CN 102758182 A CN102758182 A CN 102758182A
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matrix
layer
vapor deposition
ferrous alloy
silicon dioxide
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张新倍
陈文荣
蒋焕梧
陈正士
王莹莹
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Priority to TW100114982A priority patent/TWI490359B/zh
Priority to US13/217,950 priority patent/US8741444B2/en
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Abstract

本发明提供一种铁基合金表面镀膜方法，包括以下步骤：提供铁基合金基体；于基体上溅镀铬金属层；于铬金属层上蒸镀二氧化硅层；于二氧化硅层上蒸镀氧化铝层；于氧化铝层上蒸镀氮化硼层。本发明还提供一种由上述被方法制得的镀膜件。本发明的镀膜件具有较好高温抗氧化性能。

Description

铁基合金表面镀膜方法及由该方法其制得的镀膜件
技术领域
本发明涉及一种铁基合金表面镀膜方法及由该方法制得的镀膜件。
背景技术
铁基合金（比如模具钢）在高温下使用时，表面很容易被氧化，高温形成的不均匀氧化层不仅会降低产品的表面质量，而且铁基合金在重复使用的过程中，形成的氧化皮膜易剥落，暴露的基体在高温下将会继续被腐蚀，降低了铁基合金的使用寿命。
发明内容
有鉴于此，有必要提供一种铁基合金表面镀膜方法，使铁基合金表面具有较好的高温抗氧化性。
另外，还有必要提供一种上述镀膜方法制得的镀膜件。
一种铁基合金表面镀膜方法，包括以下步骤：
提供铁基合金基体；
于基体上溅镀铬金属层；
于铬金属层上蒸镀二氧化硅层；
于二氧化硅层上蒸镀氧化铝层；
于氧化铝层上蒸镀氮化硼层。
一种镀膜件，包括铁基合金基体，该镀膜件还包形成于基体上的铬金属层、形成于铬金属层上的二氧化硅层、形成于二氧化硅层的氧化铝层以及形成于氧化铝层上的氮化硼层。
上述镀膜件采用铬金属层做打底层，增加了整个膜层与铁基合金基体的结合力。二氧化硅层及氧化铝层熔点高，具有很好的致密性，可以阻止氧气渗入，保护基体高温下不被氧化。氮化硼层具有较好的润滑性，当镀膜件用于模具时，可以提高基体表面的流动性，易于脱模。
附图说明
图1为本发明较佳实施例的镀膜件的剖视示意图。
图2为本发明较佳实施例的铁基合金表面镀膜方法中所用溅射设备的示意图。
图3为本发明较佳实施例的铁基合金表面镀膜方法中所用蒸镀设备的示意图。
主要元件符号说明
镀膜件 10
基体 11
铬金属层 13
二氧化硅层 14
氧化铝层 15
氮化硼层 16
溅射设备 30
真空室 31
真空泵 32
气源通道 33
转架 35
铬靶 36
蒸发电源 39
蒸镀设备 40
镀膜室 41
支撑架 43
蒸镀靶材 45
如下具体实施方式将结合上述附图进一步说明本发明。
具体实施方式
本发明一较佳实施方式的铁基合金表面镀膜方法包括如下步骤：
请参阅图1，提供铁基合金基体11，该基体11的材质可以为刃具钢、模具钢、量具钢及含铬的不锈钢等。
对基体11进行去污清洗。该清洗步骤可将基体11放入盛装有乙醇或丙酮溶液的超声波清洗器中进行震动清洗，以除去基体11表面的杂质和油污等，清洗完毕后烘干备用。
请结合参阅图2，提供一溅射设备30，本实施例的溅射溅射设备30为磁控溅射镀膜机。溅射设备30包括真空室31、用以对真空室31抽真空的真空泵32以及与真空室31相通的气源通道33。该真空室31内设有转架35、铬靶36及用于控制所述溅射靶材的蒸发电源39。转架35带动基体11做圆周运行，且基体11在随转架35运行的同时也进行自转。镀膜时，溅射气体与反应气体经由气源通道33进入真空室31。
对基体11进行氩气等离子体清洗，使基体11表面进一步清洁，以提高后续镀层的附着力。该等离子体清洗过程如下：将基体11放入溅射设备30的真空室31内，将真空室31抽真空至3×10-5torr～5×10-5torr，并保持该真空度不变；然后向真空室31内通入流量为100～400sccm(标准状态毫升/分钟)的氩气(纯度为99.999%)，并施加-200～-300V的偏压于基体11，对基体11表面进行氩气等离子体清洗，清洗时间为3～20min。
在基体11上溅射铬金属层13。调节氩气流量为100~300sccm，调节偏压至-100~-300V，将基体11温度控制在20～200℃。采用直流磁控电源为蒸发电源，开启铬靶36，调节铬靶36的功率为8~12kW，对基体11溅射5~20分钟，以于基体11表面形成该铬金属层13。关闭铬靶36，取出镀覆有铬金属层13的基体11。
在铬金属层13上蒸镀二氧化硅层14。请一并参阅图3，提供一蒸镀设备40，该蒸镀设备40包括一镀膜室41、位于镀膜室41内的支撑架43及与支撑架43相对设置的蒸镀靶材45。支撑架43用于承载待镀基体11，并带动基体11做圆周运动。本实施例的蒸镀设备40采用电子束轰击的方式使蒸镀靶材45加热蒸发。
将镀覆有铬金属层13的基体11置于蒸镀设备40的镀膜室41中。对镀膜室41抽真空至4×10-5torr～6×10-5torr，并保持该真空度不变；基体11温度控制在100～200℃，向镀膜室41内通入流量为5～20sccm的氧气，以二氧化硅为蒸镀靶材，调节电子束电流值为90~120mA，以5～20nm/s的速度沉积该二氧化硅层14。沉积时间为10～30min。
继续用蒸镀法在该二氧化硅层14上沉积一层氧化铝层15。以三氧化二铝为蒸镀靶材，基体11温度控制在100～200℃，调节电子束电流值为70～100mA，控制氧气流量为15～30sccm，以5～20nm/s的速度沉积该氧化铝层15。沉积时间为10～20min。
继续用蒸镀法在该氧化铝层15上沉积一层氮化硼层16。停止向镀膜室41通入氧气，改为通入流量为15～30sccm的氮气，以氮化硼为蒸镀靶材，基体11温度控制在100～200℃，调节电子束电流值为60～90mA，以0.5～2.5nm/s的速度沉积该氮化硼层16。沉积时间为10～30min。
由此获得以铁基合金为基材的镀膜件10。
待冷却后，取出镀膜件10。
请再参阅图1，由上述铁基合金表面镀膜方法制得的镀膜件10包括基体11、形成于基体11上的铬金属层13、形成于铬金属层13上的二氧化硅层14、形成于该二氧化硅层14上的氧化铝层15以及形成形成于氧化铝层15上的氮化硼层16。
该基体11的材质可以为刃具钢、模具钢、量具钢及含铬的不锈钢等。
该铬金属层13的厚度大约为20~80nm。该二氧化硅层14的厚度大约为3～10μm。该氧化铝层15的厚度大约为3～5μm。氮化硼层16的厚度大约为600nm~3μm。
上述镀膜件10采用铬金属层13做打底层，增加了整个膜层与铁基合金基体的结合力。二氧化硅层14及氧化铝层15熔点高，具有很好的致密性，可以阻止氧气渗入，保护基体11高温下不被氧化。氮化硼层16具有较好的润滑性，当镀膜件用于模具时，可以提高基体表面的流动性，易于脱模。
上述铁基合金表面镀膜方法采用溅镀的方法沉积该与基体11直接结合的铬金属层13，使铬金属层13具有较好的结合力；而二氧化硅层14、氧化铝层15及氮化硼层16则采用蒸镀的方式沉积，且在沉积二氧化硅层14和氧化铝层过程中通入氧气，在沉积氮化硼层16过程通入氮气，以补充沉积过程中缺失的少量氧原子和氮原子，保证沉积的膜层为符合标准化学配比的化合物组成。
下面通过实施例来对本发明进行具体说明。
实施例1
本实施例所使用的基体11的材质为S316型号模具钢，溅射设备30的真空室31的真空度为3×10-5torr，蒸镀设备40的镀膜室41的真空度为5×10-5torr。
等离子体清洗：氩气流量为300sccm，基体11的偏压为-300V，等离子体清洗时间为5min。
溅镀铬金属层13：铬靶36的功率为8kW，氩气流量为150sccm，基体11的偏压为-150V，基体11温度为30℃，溅射时间为6min；该铬金属层13的厚度为25nm。
蒸镀二氧化硅层14：电子束电流值为90mA，氧气流量为5sccm，基体11的温度为120℃，沉积速率为5nm/s，沉积时间为10min；该二氧化硅层14的厚度为3μm。
蒸镀氧化铝层15：电子束电流值为70mA，氧气流量为15sccm，基体11的温度为120℃，沉积速率为5nm/s，沉积时间为10min；该氧化铝层15的厚度为3μm。
蒸镀氮化硼层16：电子束电流值为65mA，氮气流量为16sccm，基体11的温度为180℃，沉积速率为0.5nm/s，镀膜时间为20min；该氮化硼层16的厚度为600nm。
实施例2
本实施例所使用的基体11为模具，其材质为H11型号模具钢，溅射设备30的真空室31的真空度为3×10-5torr，蒸镀设备40的镀膜室41的真空度为5×10-5torr。
等离子体清洗：氩气流量为300sccm，基体11的偏压为-300V，等离子体清洗时间为5min。
溅镀铬金属层13：铬靶36的功率为10kW，氩气流量为150sccm，基体11的偏压为-150V，基体11温度为120℃，溅射时间为10min；该铬金属层13的厚度为50nm。
蒸镀二氧化硅层14：电子束电流值为110mA，氧气流量为10sccm，基体11的温度为120℃，沉积速率为10nm/s，沉积时间为15min；该二氧化硅层14的厚度为9μm。
蒸镀氧化铝层15：电子束电流值为85mA，氧气流量为20sccm，基体11的温度为120℃，沉积速率为6nm/s，沉积时间为12min；该氧化铝层15的厚度为4.3μm。
蒸镀氮化硼层16：电子束电流值为80mA，氮气流量为25sccm，基体11的温度为180℃，沉积速率为1.0nm/s，镀膜时间为30min；该氮化硼层16的厚度为1.8μm。
实施例3
本实施例所使用的基体11的材质为P20型号模具钢，溅射设备30的真空室31的真空度为3×10-5torr，蒸镀设备40的镀膜室41的真空度为5×10-5torr。
等离子体清洗：氩气流量为300sccm，基体11的偏压为-300V，等离子体清洗时间为5min。
溅镀铬金属层13：铬靶36的功率为12kW，氩气流量为150sccm，基体11的偏压为-150V，基体11温度为120℃，溅射时间为15min；该铬金属层13的厚度为78nm。
蒸镀二氧化硅层14：电子束电流值为118mA，氧气流量为19sccm，基体11的温度为120℃，沉积速率为16nm/s，沉积时间为10min；该二氧化硅层14的厚度为9.6μm。
蒸镀氧化铝层15：电子束电流值为85mA，氧气流量为20sccm，基体11的温度为120℃，沉积速率为8nm/s，沉积时间为10min；该氧化铝层15的厚度为4.8μm。
蒸镀氮化硼层16：电子束电流值为80mA，氮气流量为25sccm，基体11的温度为180℃，沉积速率为2nm/s，镀膜时间为15min；该氮化硼层16的厚度为1.8μm。
对实施例1-3制备的镀膜件10进行高温抗氧化实验。实验条件如下：在空气气氛下，将镀膜件10样品放置在高温炉内，将高温炉内的温度升温到800℃，保温1小时后取出观察，样品表面没有出现膜层的开裂、氧化、脱落等现象，说明本发明的镀膜件10高温抗氧化性能良好。

Claims (10)

1.一种铁基合金表面镀膜方法，包括以下步骤：
提供铁基合金基体；
于基体上溅镀铬金属层；
于铬金属层上蒸镀二氧化硅层；
于二氧化硅层上蒸镀氧化铝层；
于氧化铝层上蒸镀氮化硼层。
2.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：溅射所述铬金属层的步骤采用如下方式实现：采用磁控溅射法，使用铬靶，铬靶的功率为8～12kw，以氩气为溅射气体，氩气流量为100～300sccm，对基体施加偏压为-100～-300V，基体的温度为20～200℃，镀膜时间为5～20min。
3.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：蒸镀所述二氧化硅层的步骤采用如下方式实现工艺条件为：使用二氧化硅为蒸镀靶材，用电子束加热，电子束电流为90~120mA，通入流量为5～20sccm的氧气，沉积速率为5～20nm/s，基体的温度为100～200℃，沉积时间为10～30min。
4.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：蒸镀所述氧化铝层的步骤采用如下方式实现工艺条件为：使用三氧化二铝为蒸镀靶材，用电子束加热，电子束电流为70~100mA，通入流量为15～30sccm的氧气，沉积速率为5～20nm/s，基体的温度为100～200℃，沉积时间为10～20min。
5.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：蒸镀所述氮化硼层的步骤采用如下方式实现工艺条件为：使用氮化硼为蒸镀靶材，用电子束加热，电子束电流为60~90mA，基体的温度为20～200℃，沉积速度为0.5～2.5nm/s，沉积时间为10～30min。
6.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：该铁基合金表面镀膜方法还包括在溅射所述铬金属层的步骤之前，对基体进行氩气等离子体清洗。
7.如权利要求1所述的铁基合金表面镀膜方法，其特征在于：该基体的材质为刃具钢、模具钢、量具钢及含铬的不锈钢中的一种。
8.一种镀膜件，包括铁基合金基体，其特征在于：该镀膜件还包形成于基体上的铬金属层、形成于铬金属层上的二氧化硅层、形成于二氧化硅层的氧化铝层以及形成于氧化铝层上的氮化硼层。
9.如权利要求8所述的镀膜件，其特征在于：该铬金属层的厚度为20~80nm，该二氧化硅层的厚度为3～10μm，该氧化铝层的厚度为3～5μm，该氮化硼层的厚度为600nm~3μm。
10.如权利要求8所述的镀膜件，其特征在于：所述铬金属层通过磁控溅射方法形成，所述二氧化硅层、氧化铝层及氮化硼层均通过蒸镀方法形成。
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