CN102618823A - 镀膜件及其制备方法 - Google Patents
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Abstract
本发明提供一种镀膜件,其包括镁合金基体、形成于镁合金基体表面的镁层、形成于镁层表面的氮氧化镁层及形成于氮氧化镁层表面的氮化钛层。本发明镀膜件所镀膜层逐层过渡良好,膜层与镁合金基体的附着牢固;所述氮氧化镁层膜层致密,可有效延缓盐雾对镁合金基体的侵蚀,进一步提高镁合金基体的抗腐蚀性能;同时所述氮化钛层可有效避免所述氮氧化镁层的磨损刮擦,有效提高镀膜件的使用寿命。此外,本发明还提供一种上述镀膜件的制备方法。
Description
技术领域
本发明涉及一种镀膜件及该镀膜件的制备方法。
背景技术
镁合金具有质量轻、散热性能好等优点,在通讯、电子、交通运输、建筑及航天航空等领域应用广泛。然而由于镁合金的化学活性较高,在空气中很容易氧化,生成疏松、保护能力差的氧化膜,导致镁合金在含有电解质的湿气中,例如海洋表面大气环境,表面容易出现严重的腐蚀,从而破环镁合金制品的外观,同时导致制品使用寿命缩短。
耐盐雾侵蚀性能是镁合金耐腐蚀性能的一个重要参数,为了提高镁合金的耐盐雾侵蚀性能,通常需要对镁合金表面进行表面镀膜处理。真空镀膜(PVD)技术虽是一种非常环保的镀膜工艺,且可镀制的膜层种类丰富、耐磨性能优异,但PVD工艺沉积的薄膜往往是以柱状晶形态生长,因此膜层存在大量的晶间间隙,导致薄膜致密性不够而无法有效地延缓盐雾的侵蚀。
发明内容
有鉴于此,有必要提供一种可有效提高镁合金耐盐雾侵蚀性能的镀膜件。
另外,还有必要提供一种上述镀膜件的制备方法。
一种镀膜件,其包括镁合金基体、形成于镁合金基体表面的镁层、形成于镁层表面的氮氧化镁层及形成于氮氧化镁层表面的氮化钛层。
一种镀膜件的制备方法,其包括如下步骤:
提供一镁合金基体;
以镁靶为靶材,采用磁控溅射法在镁合金基体表面形成一镁层;
以镁靶为靶材,以氧气和氮气为反应气体,采用磁控溅射法在该镁层表面形成一氮氧化镁层;
以钛靶为靶材,采用磁控溅射法在该氮氧化镁层表面形成一氮化钛层。
本发明镀膜件所镀膜层逐层过渡良好,膜层与镁合金基体的附着牢固;所述氮氧化镁层由比较细小的晶粒组成,晶间间隙比较小,膜层非常致密,可有效延缓盐雾对镁合金基体的侵蚀,进一步提高镁合金基体的抗腐蚀性能;同时所述氮化钛层具有较高的硬度和耐磨性,可有效避免所述氮氧化镁层的磨损刮擦,有效提高镀膜件的使用寿命。
附图说明
图1为本发明一较佳实施例镀膜件的剖视图;
图2为本发明一较佳实施例真空镀膜机的俯视示意图。
主要元件符号说明
镀膜件 10
镁合金基体 11
镁层 13
氮氧化镁层 15
氮化钛层 17
真空镀膜机 20
镀膜室 21
镁靶 23
钛靶 24
轨迹 25
真空泵 30
具体实施方式
请参阅图1,本发明一较佳实施方式的镀膜件10包括镁合金基体11、形成于镁合金基体11表面的镁层13、形成于镁层13表面的氮氧化镁(MgON)层15及形成于氮氧化镁层15表面的氮化钛(TiN)层17。
该镁层13可以磁控溅射的方式形成,其厚度为20~50nm。所述镁层13可充当打底层的作用,使膜层与镁合金基体11附着更牢固。
该氮氧化镁层15可以磁控溅射的方式形成,其厚度为200~300nm。该氮氧化镁层15由细小的纳米晶粒组成,晶间间隙比较小,膜层非常致密。该氮氧化镁层15中镁的原子百分含量为25%~40%,氧的原子百分含量为25%~40%,氮的原子百分含量为20%~35%。
该氮化钛层17可以磁控溅射的方式形成,其厚度可为100~200nm。氮化钛层17具有较高的硬度和耐磨性,可有效保护氮氧化镁层15,使其免受磨损、刮擦。所述氮化钛层17也可根据实际需要替换成其它的具有较高的硬度和耐磨性的膜层。
本发明一较佳实施方式的镀膜件10的制备方法,其包括以下步骤:
(a)提供镁合金基体11。
(b)将镁合金基体11放入无水乙醇中进行超声波清洗,以去除镁合金基体11表面的污渍,清洗时间可为5~20min。
(c)对经上述处理后的镁合金基体11的表面进行氩气等离子体清洗,以进一步去除镁合金基体11表面的油污,以及改善镁合金基体11表面与后续镀层的结合力。结合参阅图2,提供一真空镀膜机20,该真空镀膜机20包括一镀膜室21及连接于镀膜室21的一真空泵30,真空泵30用以对镀膜室21抽真空。该镀膜室21内设有转架(未图示)、相对设置的二镁靶23及相对设置的二钛靶24。转架带动镁合金基体11沿圆形的轨迹25公转,且镁合金基体11在沿轨迹25公转时亦自转。
该等离子体清洗的具体操作及工艺参数可为:如图2所示,将镁合金基体11固定于真空镀膜机20的镀膜室21的转架上,将该镀膜室21抽真空至3×10-3Pa,然后向镀膜室21内通入流量为500sccm(标准状态毫升/分钟)的氩气(纯度为99.999%),并施加-200~-500V的偏压于镁合金基体11,对镁合金基体11表面进行氩气等离子体清洗,清洗时间为3~10min。
(d)采用磁控溅射法在经氩气等离子体清洗后的镁合金基体11上溅镀镁层13。溅镀该镁层13在所述真空镀膜机20中进行,抽真空使该镀膜室21的本底真空度为3×10-3Pa,加热该镀膜室21至温度为80~200℃;开启二镁靶23,设置镁靶23的功率为3~10kW,设定施加于镁合金基体11的偏压为-100~-300V;通入工作气体氩气,氩气的流量为100~300sccm,镀膜时间为10~30min。该镁层13的厚度为20~50nm。
(e)继续采用磁控溅射法在所述镁层13的表面溅镀氮氧化镁层15。溅镀该氮氧化镁层15时通入氧气和氮气为反应气体,氧气流量为80~120sccm,氮气流量为50~80sccm,其他工艺参数与沉积所述镁层13的相同,镀膜时间为60~90min。该氮氧化镁层15的厚度为200~300nm。
(f)继续采用磁控溅射法在所述氮氧化镁层15的表面形成氮化钛层17。关闭二镁靶23,开启二钛靶24,设置钛靶24的功率为3~10kW,设定施加于镁合金基体11的偏压为-100~-300V;通入氮气为反应气体,氮气流量为50~80sccm,通入工作气体氩气,氩气的流量为100~300sccm,镀膜时间为30~60min。该氮化钛层17的厚度为100~200nm。
下面通过实施例来对本发明进行具体说明。
实施例1
本实施例所使用的真空镀膜机20为中频磁控溅射镀膜机。
等离子体清洗:氩气流量为500sccm,镁合金基体11的偏压为-500V,等离子体清洗时间为5min。
溅镀镁层13:氩气流量为100sccm,镁靶23的功率为3kW,镁合金基体11的偏压为-100V,镀膜温度为80℃,镀膜时间为10min;该镁层13的厚度为20nm。
溅镀氮氧化镁层15:氧气流量为80sccm,氮气流量为50sccm,其他工艺参数与沉积所述镁层13的相同,镀膜时间为60min,该氮氧化镁层15的厚度为200nm。
溅镀氮化钛层17:氮气流量为50sccm,氩气流量为100sccm,钛靶24的功率为3kW,镁合金基体11的偏压为-100V,镀膜时间为30min,该氮化钛层17的厚度为100nm。
实施例2
本实施例所使用的真空镀膜机20与实施例1中的相同。
等离子体清洗:氩气流量为500sccm,镁合金基体11的偏压为-500V,等离子体清洗时间为5min。
溅镀镁层13:氩气流量为300sccm,镁靶23的功率为10kW,镁合金基体11的偏压为-300V,镀膜温度为200℃,镀膜时间为30min;该镁层13的厚度为50nm。
溅镀氮氧化镁层15:氧气流量为120sccm,氮气流量为80sccm,其他工艺参数与沉积所述镁层13的相同,镀膜时间为90min,该氮氧化镁层15的厚度为300nm。
溅镀氮化钛层17:氮气流量为80sccm,氩气流量为300sccm,钛靶24的功率为10kW,镁合金基体11的偏压为-300V,镀膜时间为60min,该氮化钛层17的厚度为200nm。
盐雾测试
对由本发明的方法所制备的镀膜件10进行35℃中性盐雾(NaCl浓度为5%)测试。结果发现,由本发明实施例1、2的方法所制备的镀膜件10均在72小时后才出现有腐蚀现象。
本发明镀膜件10在所述镁合金基体11的表面依次沉积镁层13、氮氧化镁层15及氮化钛层17,所镀膜层逐层过渡良好,膜层与镁合金基体11的附着牢固;所述氮氧化镁层15由比较细小的晶粒组成,晶间间隙比较小,膜层非常致密,可有效延缓盐雾对镁合金基体11的侵蚀,进一步提高镁合金基体11的抗腐蚀性能;同时所述氮化钛层17具有较高的硬度和耐磨性,可有效避免所述氮氧化镁层15的磨损刮擦,有效提高镀膜件10的使用寿命。
Claims (9)
1.一种镀膜件,其包括镁合金基体,其特征在于:该镀膜件还包括形成于镁合金基体表面的镁层、形成于镁层表面的氮氧化镁层及形成于氮氧化镁层表面的氮化钛层。
2.如权利要求1所述的镀膜件,其特征在于:该氮氧化镁层中镁的原子百分含量为25%~40%,氧的原子百分含量为25%~40%,氮的原子百分含量为20%~35%。
3.如权利要求1所述的镀膜件,其特征在于:该镁层以磁控溅射的方式形成,其厚度为20~50nm。
4.如权利要求1所述的镀膜件,其特征在于:该氮氧化镁层以磁控溅射的方式形成,其厚度为200~300nm。
5.如权利要求1所述的镀膜件,其特征在于:该氮化钛层以磁控溅射的方式形成,其厚度为100~200nm。
6.一种镀膜件的制备方法,其包括如下步骤:
提供一镁合金基体;
以镁靶为靶材,采用磁控溅射法在镁合金基体表面形成一镁层;
以镁靶为靶材,以氧气和氮气为反应气体,采用磁控溅射法在该镁层表面形成一氮氧化镁层;
以钛靶为靶材,采用磁控溅射法在该氮氧化镁层表面形成一氮化钛层。
7.如权利要求6所述的镀膜件的制备方法,其特征在于:所述形成镁层的步骤的具体工艺参数为:镁靶的功率为3~10kW,以氩气为工作气体,氩气的流量为100~300sccm,镁合金基体的偏压为-100~-300V,镀膜温度为80~200℃,镀膜时间为10~30min。
8.如权利要求6所述的镀膜件的制备方法,其特征在于:所述形成氮氧化镁层的步骤的具体工艺参数为:镁靶的功率为3~10kW,氧气流量为80~120sccm,氮气流量为50~80sccm,以氩气为工作气体,氩气的流量为100~300sccm,镁合金基体的偏压为-100~-300V,镀膜温度为80~200℃,镀膜时间为60~90min。
9.如权利要求6所述的镀膜件的制备方法,其特征在于:所述形成氮化钛层的步骤的具体工艺参数为:钛靶的功率为3~10kW,氮气流量为50~80sccm,以氩气为工作气体,氩气的流量为100~300sccm,镁合金基体的偏压为-100~-300V,镀膜温度为80~200℃,镀膜时间为30~60min。
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CN104195517A (zh) * | 2014-08-29 | 2014-12-10 | 南京工程学院 | 一种降低生物医用镁合金表面涂层残余应力的方法 |
CN104213091A (zh) * | 2014-08-29 | 2014-12-17 | 南京工程学院 | 改善生物医用镁合金表面磁控溅射TiN涂层结合性能的方法 |
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CN108474107B (zh) * | 2016-05-16 | 2020-06-12 | 株式会社爱发科 | 内部应力控制膜的形成方法 |
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DE102004044919A1 (de) * | 2004-09-14 | 2006-03-30 | Martin Balzer | Dekorative Beschichtung zum Korrosionsschutz auf Basis von Refraktärmetall-Magnesium-Nitriden sowie Verfahren zur Herstellung derselben |
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JP4167468B2 (ja) * | 2002-10-08 | 2008-10-15 | 新日本製鐵株式会社 | 金属板表面処理剤、張り剛性に優れた表面処理金属板およびその製造方法ならびに高剛性パネル |
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US6159618A (en) * | 1997-06-10 | 2000-12-12 | Commissariat A L'energie Atomique | Multi-layer material with an anti-erosion, anti-abrasion, and anti-wear coating on a substrate made of aluminum, magnesium or their alloys |
DE102004044919A1 (de) * | 2004-09-14 | 2006-03-30 | Martin Balzer | Dekorative Beschichtung zum Korrosionsschutz auf Basis von Refraktärmetall-Magnesium-Nitriden sowie Verfahren zur Herstellung derselben |
CN101119860A (zh) * | 2005-02-17 | 2008-02-06 | 桑德维克知识产权股份公司 | 涂敷的金属产品、其制备方法及该方法的用途 |
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CN104195517A (zh) * | 2014-08-29 | 2014-12-10 | 南京工程学院 | 一种降低生物医用镁合金表面涂层残余应力的方法 |
CN104213091A (zh) * | 2014-08-29 | 2014-12-17 | 南京工程学院 | 改善生物医用镁合金表面磁控溅射TiN涂层结合性能的方法 |
CN104213091B (zh) * | 2014-08-29 | 2017-04-12 | 南京工程学院 | 改善生物医用镁合金表面磁控溅射TiN涂层结合性能的方法 |
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