CN103302916A - 镀膜件及其制备方法 - Google Patents

镀膜件及其制备方法 Download PDF

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CN103302916A
CN103302916A CN201210070120XA CN201210070120A CN103302916A CN 103302916 A CN103302916 A CN 103302916A CN 201210070120X A CN201210070120X A CN 201210070120XA CN 201210070120 A CN201210070120 A CN 201210070120A CN 103302916 A CN103302916 A CN 103302916A
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silicon
metallic matrix
film
carburizing
coated part
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CN103302916B (zh
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曹达华
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Haining Economic Development Industrial Park Development and Construction Co., Ltd
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Shenzhen Futaihong Precision Industry Co Ltd
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Abstract

本发明提供一种镀膜件，包括金属基体，该镀膜件还包括形成于该金属基体表层的渗碳-硅层、形成于该渗碳-硅层上的结合层以及形成于该结合层上的颜色层，该渗碳-硅层是通过对金属基体进行真空离子渗碳-硅处理而于金属基体表层渗入碳、硅元素而形成，该结合层由金属形成，该颜色层由金属元素与非金属元素组成。本发明还提供一种上述镀膜件的制备方法。

Description

镀膜件及其制备方法
技术领域
本发明涉及一种镀膜件及其制备方法，尤其涉及一种具有较高硬度的装饰膜的镀膜件及其制备方法。
背景技术
物理气相沉积（PVD）由于比较环保，而且制备的膜层具有金属质感以及较好的附着性，因此被广泛用于在计算机、通信和消费类电子产品的金属外壳上制备装饰性膜层。然而，消费者除了对这些产品的外壳的装饰性有较高的要求外，对外壳的表面硬度及耐磨性要求也越来越高。一般装饰性PVD膜层的厚度为2-4微米，经PVD镀膜处理的外壳表面，其复合硬度通常只有HV600，若要进一步提高硬度，通常需要增加膜层厚度。然而，随着膜层沉积厚度的增加，不仅增加成本，而且膜层过厚容易导致膜层表面发朦，光亮度降低，颜色异常。所以，单独的PVD工艺难以满足这种需求。
发明内容
有鉴于此，本发明提供一种具有较高硬度的装饰膜的镀膜件。
另外，本发明还提供一种上述镀膜件的制备方法。
一种镀膜件，包括金属基体，该镀膜件还包括形成于该金属基体表层的渗碳-硅层、形成于该渗碳-硅层上的结合层以及形成于该结合层上的颜色层，该渗碳-硅层是通过对金属基体进行真空离子渗碳-硅处理而于金属基体表层渗入碳、硅元素而形成，该结合层由金属形成，该颜色层由金属元素与非金属元素组成。
一种镀膜件的制备方法，包括对金属基体进行真空离子渗碳-硅处理，以于该金属基体的表层渗入碳、硅元素而形成一渗碳-硅层，以及采用磁控溅射方法在该渗碳-硅层上依次沉积一结合层及一颜色层，其中，
沉积该结合层是在溅射条件下，以铬、钛及锆中的一种为靶材，在靶材上施加电源使靶材物质溅射并沉积到渗碳-硅层表面；
沉积该颜色层是在溅射条件下，以铬或钛为靶材，以乙炔、氧气及氮气中的一种或多种为反应气体，在靶材上施加电源是靶材物质溅射并沉积到结合层表面。
上述镀膜件的制备方法先采用碳和硅共渗于金属基体表层获得该渗碳-硅层，由于碳和硅同属IVA族，具有很多相似的性质，易形成SiC、Si及C的共渗，而且SiC的硬度接近金刚石的硬度，因此，该渗碳-硅层可以为后续膜层（结合层及颜色层）提供更硬的基底，从而可以是镀膜件获得更高的表面复合硬度。
本发明通过C及Si离子共渗处理配合PVD镀膜工艺，在不增加PVD膜层厚度、膜层表面不发朦的基础上，使镀膜件的耐磨性及耐刮伤性能获得较大提高。
附图说明
图1是本发明一较佳实施例镀膜件的剖视图。
图2是图1所示镀膜件的制备过程中所用真空离子渗碳-硅设备渗碳-硅设备的结构示意图。
主要元件符号说明
镀膜件 10
金属基体 11
渗碳-硅层 13
结合层 14
颜色层 15
真空离子渗碳-硅设备 20
真空炉 21
加热器 22
离子源 23
真空泵 25
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
请参阅图1，本发明较佳实施例的镀膜件10包括金属基体11、形成于金属基体11上的渗碳-硅层13、形成于渗碳-硅层13上的结合层14及形成于结合层14的颜色层15。
金属基体11可为不锈钢，还可为钛合金、铝合金等金属。
该渗碳-硅层13通过对金属基体11的表层进行真空离子渗碳-硅处理形成。该渗碳-硅层13中碳元素的质量百分含量比金属基体11中碳元素的质量百分含量高0.12%-0.42%，渗碳-硅层13中硅元素的质量百分含量比金属基体11中硅元素的质量百分含量高0.05%-0.3%。渗碳-硅层13的厚度为0.1mm-0.3mm。
该结合层14为铬、钛或锆等结合力较强、与金属基体11热膨胀系数相近的金属形成。结合层14主要用于提高颜色层15的附着力。当金属基体11为不锈钢时，结合层14优选为铬。结合层14的厚度可为0.1μm-0.3μm。
该颜色层15由金属元素与非金属元素组成，其主要为镀膜件10提供装饰性的外观。为了使颜色层15具有较高的耐磨性，颜色层15还应当具有较高的硬度。比如，该颜色层15可为碳化铬、氮化铬、氮氧化铬、碳化钛、氮化钛及氮碳化钛中的一种。
在本发明一实施例中，该颜色层15由碳元素与铬元素组成。颜色层15中碳元素与铬元素的原子个数比大约为1:（0.3-1），且颜色层15中碳元素的质量百分含量由靠近结合层14至远离结合层14的方向呈梯度增加。颜色层15的厚度可为2.0μm-2.5μm。
所述结合层14与颜色层15可分别通过磁控溅射方法形成。
上述镀膜件10的制备方法，主要包括对金属基体11的表层进行真空离子渗碳-硅处理形成该渗碳-硅层13，以及采用磁控溅射方法在该渗碳-硅层13上依次沉积该结合层14及该颜色层15。
所述真空离子渗碳-硅处理是在一真空离子渗碳-硅设备20（如图2所示）中进行。该真空离子渗碳-硅设备20包括一真空炉21、用于使金属基体11升温的加热器22、设置于真空炉21内的一离子源23以及用以对真空炉21抽真空的真空泵25。所述离子源23用于将渗碳-硅气体电离，向真空炉21提供含碳离子及硅离子的离化气体。
真空离子渗碳-硅处理时，将金属基体11放置于真空炉21中，开启真空泵25，将真空炉21排气至压强为0.1Pa-1.0Pa，然后开启加热器22使金属基体11升温至450℃-600℃，向离子源23充入渗碳气体甲烷（CH4）、渗硅气体硅烷(SiH4)及惰性气体氩气。甲烷、硅烷及氩气之间的流量比为(1-2):(1-2):(2-3)。甲烷及硅烷被离子源23电离成为离化气体进入真空炉21，使真空炉21内气压为0.5Pa-2.5Pa。离化气体中的碳离子与硅离子冲击金属基体11而进入金属基体11表层，由此于金属基体11表层形成该渗碳-硅层13。真空离子渗碳-硅处理的时间为180min-300min。然后向真空炉21充入冷却气体（如氩气）对金属基体11进行冷却。充入冷却气体后真空炉21内压力为1.0atm-2.0atm。经大约20min-40min后，取出金属基体11。
沉积该结合层14是在溅射条件下，以铬、钛及锆中的一种为靶材，在靶材上施加电源使靶材物质溅射并沉积到渗碳-硅层13表面形成结合层14。
沉积该颜色层15是在溅射条件下，以铬或钛为靶材，以乙炔（C2H2）、氧气（O2）及氮气（N2）中的一种或多种为反应气体，在靶材上施加电源是靶材物质溅射并沉积到结合层14表面形成该颜色层15。
所述的磁控溅射条件包括以惰性气体为溅射气体，该惰性气体可以为氩气，其流量可为150sccm(标准状态毫升/分钟)-250sccm；镀膜压力（即镀膜时镀膜室内的绝对压力）为0.3Pa-0.6Pa；镀膜温度为130℃-180℃。
所述电源可以为现有的各种用于磁控溅射镀膜的电源，优选为中频电源。
下面以结合层14为铬层、颜色层15由碳元素与铬元素组成为例，对本发明进行进一步详细说明。
实施例1
1. 超声清洗
将304不锈钢材质的金属基体11放入乙醇溶液中进行超声波清洗，以除去金属基体11表面的杂质和油污等，清洗完毕后烘干备用。
2. 真空离子渗碳-硅处理
将金属基体11放入真空离子渗碳-硅设备20的真空炉21中，开启真空泵25，将真空炉21排气至压强为0.1Pa，然后开启加热器22使金属基体11升温至450℃，向离子源23充入渗碳气体甲烷、渗硅气体硅烷及氩气。甲烷、硅烷及氩气之间的流量比为1:1:2，使真空炉21内气压为0.5Pa。真空离子渗碳-硅处理的时间为180min，于金属基体11表层形成一渗碳-硅层13。然后向真空炉21充入冷却气体氩气，使真空炉21内压力为1.0atm。经大约20min后，取出金属基体11。
2. PVD镀膜
采用磁控溅射设备（深圳南方创新真空技术有限公司生产，型号为SM-1100H）。该磁控溅射设备包括真空室、转架、磁控靶和偏压电源。磁控靶为对靶结构，包括两对铬靶，每对靶之间形成有一定距离。基体固定在转架上，转架旋转时带动基体从每对铬靶之间经过。
洗靶：将真空室中绝对压力调至6.0×10-3Pa，然后向真空室通入氩气直至压力为0.8Pa，开启铬靶的电源，调节电源功率为8kW，对铬靶辉光清洗8分钟。
离子清洗基体：关闭铬靶的电源，调节真空室压力为0.6Pa，对金属基体11施加-1000V的偏压，对金属基体11进行氩气等离子体清洗15分钟。
溅射结合层14：向真空室通入氩气，氩气流量为150sccm，控制真空室内压力为0.3Pa，调节真空室内温度为130℃，开启铬靶的电源，调节电源功率为10kW，调节施加于金属基体11上的偏压为-100V，对金属基体11溅射15分钟，以于金属基体11表面形成所述由铬金属形成的结合层14。结合层14的厚度为0.25μm。
溅射颜色层15：维持上述操作，不同的是，调节铬靶的电源功率为11kW，同时通入反应气体乙炔，乙炔的初始流量为50sccm，在沉积颜色层15的过程中，每4min将乙炔的流量增大1sccm，当氮气的流量到达80sccm时，停止增大乙炔流量，由此在结合层14上沉积该由碳元素与铬元素组层，且碳元素含量随厚度递增的颜色层15。溅射颜色层15的时间为120分钟。颜色层15的厚度为2.4μm。
关闭铬靶、偏压电源并停止通入乙炔，冷却后取出镀覆好的金属基体11，肉眼观察颜色层15无发朦等颜色异常。
实施例1的样品记做S1。
实施例2
1. 超声清洗
将304不锈钢材质的金属基体11放入乙醇溶液中进行超声波清洗，以除去金属基体11表面的杂质和油污等，清洗完毕后烘干备用。
2. 真空离子渗碳-硅处理
将金属基体11放入真空离子渗碳-硅设备20的真空炉21中，开启真空泵25，将真空炉21排气至压强为1.0Pa，然后开启加热器22使金属基体11升温至600℃，向离子源23充入渗碳气体甲烷、渗硅气体硅烷及氩气。甲烷、硅烷及氩气之间的流量比为2:2:3，使真空炉21内气压为2.0Pa。真空离子渗碳-硅处理的时间为300min，于金属基体11表层形成一渗碳-硅层13。然后向真空炉21充入冷却气体氩气，使真空炉21内压力为2.0atm。经大约40min后，取出金属基体11。
2. PVD镀膜
采用磁控溅射设备（深圳南方创新真空技术有限公司生产，型号为SM-1100H）。该磁控溅射设备包括真空室、转架、磁控靶和偏压电源。磁控靶为对靶结构，包括两对铬靶，每对靶之间形成有一定距离。基体固定在转架上，转架旋转时带动基体从每对铬靶之间经过。
洗靶：将真空室中绝对压力调至5.0×10-3Pa，然后向真空室通入氩气直至压力为1.0Pa，开启铬靶的电源，调节电源功率为12kW，对铬靶辉光清洗2分钟。
离子清洗基体：关闭铬靶的电源，调节真空室压力为0.6Pa，对金属基体11施加-1100V的偏压，对金属基体11进行氩气等离子体清洗20分钟。
溅射结合层14：向真空室通入氩气，氩气流量为200sccm，控制真空室内压力为0.7Pa，调节真空室内温度为180℃，开启铬靶的电源，调节电源功率为18kW，调节施加于金属基体11上的偏压为-150V，对金属基体11溅射5分钟，以于金属基体11表面形成所述由铬金属形成的结合层14。结合层14的厚度为0.2μm。
溅射颜色层15：维持上述操作，不同的是，调节铬靶的电源功率为19kW，同时通入反应气体乙炔，乙炔的初始流量为60sccm，在沉积颜色层15的过程中，每2min将乙炔的流量增大1sccm，当氮气的流量到达90sccm时，停止增大乙炔流量，由此在结合层14上沉积该由碳元素与铬元素组层，且碳元素含量随厚度递增的颜色层15。溅射颜色层15的时间为60分钟。颜色层15的厚度为2.2μm。
关闭铬靶、偏压电源并停止通入乙炔，冷却后取出镀覆好的金属基体11，肉眼观察颜色层15无发朦等颜色异常。
实施例2的样品记做S2。
对比例1
该对比例中，除了未对金属基体进行真空离子渗碳-硅处理之外，其它均与实施例1相同。对比例的样品记做D1。
对比例2
该对比例中，除了未对金属基体进行真空离子渗碳-硅处理之外，其它均与实施例2相同。对比例的样品记做D2。
测试
使用下面的方法对实施例1-2及对比例1-2的样品的维氏硬度、铅笔硬度及耐弹簧力（Rod Scrach Test）进行了测试。所述三种测试测试的标准已经为业界熟知，所以不再列出。测试结果如下表所示：
样品编号 维氏硬度 铅笔硬度 耐弹簧力
S1 806HV ≧6H 20N，未露出基体
D1 578HV 4H 20N，露出基体
S2 815HV ≧6H 20N，未露出基体
D2 580HV 4H 20N，露出基体
由测试结果可知，在对金属基体11进行PVD镀膜前，对金属基体11进行真空离子渗碳-硅处理可使镀膜件10的表面复合硬度及耐刮伤性获得明显提高。
本发的镀膜件10可为笔记型计算机、个人数字助理等电子装置的壳体，或为其它装饰类产品的壳体。
上述镀膜件10的制备方法先采用碳和硅共渗于金属基体11表层获得一渗碳-硅层13，由于碳和硅同属IVA族，具有很多相似的性质，易形成SiC、Si及C的共渗，而且SiC的硬度接近金刚石的硬度，因此，该渗碳-硅层13可以为后续膜层（结合层14及颜色层15）提供更硬的基底，从而可以是镀膜件10获得更高的表面复合硬度。
本发明通过C及Si离子共渗处理配合PVD镀膜工艺，在不增加PVD膜层厚度、膜层表面不发朦的基础上，使镀膜件10的耐磨性及耐刮伤性能获得较大提高。

Claims (10)

1.一种镀膜件，包括金属基体，其特征在于：该镀膜件还包括形成于该金属基体表层的渗碳-硅层、形成于该渗碳-硅层上的结合层以及形成于该结合层上的颜色层，该渗碳-硅层是通过对金属基体进行真空离子渗碳-硅处理而于金属基体表层渗入碳、硅元素而形成，该结合层由金属形成，该颜色层由金属元素与非金属元素组成。
2.如权利要求1所述的镀膜件，其特征在于：该渗碳-硅层中碳元素的质量百分含量比金属基体中碳元素的质量百分含量高0.12%-0.42%，硅元素的质量百分含量比金属基体中硅元素的质量百分含量高0.05%-0.3%。
3.如权利要求1所述的镀膜件，其特征在于：该渗碳-硅层的厚度为0.1mm-0.3mm。
4.如权利要求1所述的镀膜件，其特征在于：该金属基体为不锈钢，该结合层为铬。
5.如权利要求4所述的镀膜件，其特征在于：该颜色层由碳元素与铬元素组成，颜色层中碳元素与铬元素的原子个数比为1:（0.3-1），且颜色层中碳元素的质量百分含量由靠近结合层至远离结合层的方向呈梯度增加。
6.如权利要求1所述的镀膜件，其特征在于：该颜色层为氮化铬、氮氧化铬、碳化钛、氮化钛及氮碳化钛中的一种。
7.如权利要求1所述的镀膜件，其特征在于：该颜色层通过磁控溅射方法形成。
8.一种镀膜件的制备方法，包括对金属基体进行真空离子渗碳-硅处理，以于该金属基体的表层渗入碳、硅元素而形成一渗碳-硅层，以及采用磁控溅射方法在该渗碳-硅层上依次沉积一结合层及一颜色层，其中，
沉积该结合层是在溅射条件下，以铬、钛及锆中的一种为靶材，在靶材上施加电源使靶材物质溅射并沉积到渗碳-硅层表面；
沉积该颜色层是在溅射条件下，以铬或钛为靶材，以乙炔、氧气及氮气中的一种或多种为反应气体，在靶材上施加电源是靶材物质溅射并沉积到结合层表面。
9.如权利要求8所述的镀膜件的制备方法，其特征在于：该真空离子渗碳-硅处理包括：将金属基体放置于一真空炉中，将真空炉抽真空至压强为0.1Pa-1.0Pa，并将金属基体升温至450℃-600℃，向真空炉充入含碳离子及硅离子的离化气体，使真空炉内气压为0.5Pa-2.5Pa，所述碳离子与硅离子冲击金属基体而进入金属基体表层，由此于金属基体表层形成该渗碳-硅层，该真空离子渗碳-硅处理的时间为180min-300min。
10.如权利要求8所述的镀膜件的制备方法，其特征在于：所述磁控溅射条件包括以惰性气体为溅射气体，溅射气体的流量为150sccm-250sccm；镀膜压力为0.3Pa-0.6Pa；镀膜温度为130℃-180℃。
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CN107313007B (zh) * 2017-05-23 2019-02-05 林育周 一种充电接头、电子设备及充电接头强化方法
CN108330432A (zh) * 2018-03-03 2018-07-27 西北有色金属研究院 一种钢材表面无氢复合改性层的制备方法
CN111349889A (zh) * 2019-11-29 2020-06-30 森科五金(深圳)有限公司 一种黑色绝缘涂层及其制作方法
CN111349889B (zh) * 2019-11-29 2022-07-01 森科五金(深圳)有限公司 一种黑色绝缘涂层及其制作方法

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