CN110938851A - 一种耐指纹哑金复合镀层的制备方法 - Google Patents
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Abstract
本发明公开了一种耐指纹哑金复合镀层的制备方法,方法包括对基材进行电镀前处理后,采用电镀技术依次在基底材料上电镀打底铜层、焦磷酸铜层、硫酸铜层和水雾镍层,再对水雾镍层精洗后,结合PVD技术沉积氮化锆层,进而实现得到一种哑金L值在75~85范围内,可控性强,能耐指纹、高应力的哑金镀层复合材料。该制备工艺简单、环保、生产周期短、成本低,具有非常好的应用价值。
Description
技术领域
本发明涉及的是材料技术领域,具体涉及一种耐指纹哑金复合镀层的制备方法。
背景技术
在卫浴等工业产品上,为了美观、防锈、防耐磨等用途,往往会在产品上进行镀层。金色因具备高贵、时尚、漂亮等特点,其在人们生活中有越来越多的应用,比如卫浴花洒、水槽、水龙头等进行镀层呈现出金色,既美观又有各种实用用途。而卫浴用产品表面金色镀层通常是金镀层或金色的金属化合物。
目前,对于卫浴用产品的金色镀层主要采用电镀直接镀金和PVD镀金两种技术。电镀直接镀金由于容易产生含重金属离子的电镀废水和各类酸雾废气,不但成本高、污染大、对生产人员身体健康构成很大威胁;PVD(Physical Vapor Deposition)也叫物理气相沉积,通常把真空蒸镀、溅射镀膜、离子镀等都称为物理气相沉积。PVD镀金的镀金层光亮、方法本身简单、快速、环保,但是往往镀层应力小,容易掉色。CN108611667A申请公开了一种铜合金基材上环保复合镀层及其制备,在铜合金基材表面电镀铜层、镍腐蚀光亮层、和三价铬环保层,再结合PVD技术沉积形成CrAlTiC钝化层。然而,此申请的电镀铜层时采用酸铜,铜合金基材只能采用铜基,对基材的要求非常有局限性;其次,此申请最后制备得到的镀层为光亮的复合镀金。
当镀层表面由于光亮,虽然美观,但同时当经多次触摸后,例如水龙头等需要经常触摸时,镀层表面容易形成指纹接触污染,影响美观。因此,提供一种能适用于大多数基材,且环保、耐指纹、高应力的金色镀层复合材料及其制备方法非常有实用价值和经济价值。
发明内容
本发明的目的在于提供一种在基底材料上电镀铜层和高哑度的水雾镍,然后在水雾镍层上PVD技术沉积氮化锆层,进而实现环保、耐指纹、高应力的金色镀层复合材料的制备方法。
为了实现上述目的,本发明通过以下技术方案:
一方面,本发明提供一种耐指纹哑金复合镀层的制备方法,所述制备方法包括以下步骤:
(1)将金属基材表面清洗干净,进行电镀前处理,包括镜面抛光处理和清洗处理;
(2)在步骤1处理后的洁净基材上电镀铜层,包括依次电镀打底铜层、焦磷酸铜层和硫酸铜层;
(3)在步骤2制得的洁净硫酸铜层上电镀水雾镍层;
(4)对步骤3制得的水雾镍层进行清洗;
(5)在步骤4处理后的洁净水雾镍层上PVD镀氮化锆层。
进一步地,步骤1中抛光处理包括开皮、研磨、整平和镜面精抛工艺;基材清洗处理分别通过超声波除蜡、超声波除油、电解和纯水清洗过程。
进一步地,步骤2中打底铜的电镀液为氰化亚铜浓度50g/L~65g/L,游离氰化钠浓度17g/L~25g/L;其工艺条件为:温度30℃~60℃,pH值11.5~13,电压2V~5V,电流50A~150A,时间1200s~1800s;
更进一步地,打底铜的电镀液为氰化亚铜浓度55g/L~60g/L,游离氰化钠浓度18g/L~22g/L;其工艺条件为:温度30℃~60℃,pH值11.5~13,电压2V~5V,电流50A~100A,时间1200s~1500s;
进一步地,步骤2中焦磷酸铜的电镀液为焦磷酸钾浓度300g/L~400g/L,焦磷酸铜浓度40g/L~50g/L,氨水浓度5mL/L~7mL/L,其工艺条件为:温度40℃~50℃,pH值7~9,电压1.5V~5V,电流50A~100A,时间800s~1500s;
更进一步地,焦磷酸铜的电镀液为焦磷酸钾浓度320g/L~380g/L,焦磷酸铜浓度40g/L~45g/L,氨水浓度5mL/L~7mL/L,其工艺条件为:温度40℃~50℃,pH值7~9,电压2V~4V,电流50A~100A,时间800s~1200s;
进一步地,步骤2中硫酸铜的电镀液为五水合硫酸铜浓度250g/L~300g/L,硫酸浓度50g/L~60g/L,其工艺条件为:温度30℃~50℃,pH值7~9,电压2V~6V,电流200A~400A,时间3000s~6000s;
更进一步地,硫酸铜的电镀液为五水合硫酸铜浓度250g/L~280g/L,硫酸浓度50g/L~60g/L,其工艺条件为:温度35℃~40℃,pH值7~9,电压2V~6V,电流250A~300A,时间3000s~4500s;
进一步地,步骤3中水雾镍层的电镀液为硫酸镍浓度200g/L~400g/L,氯化镍浓度50g/L~70g/L,硼酸浓度25g/L~35g/L,镍S-A添加剂浓度15mL/L~25mL/L,镍S-B添加剂浓度15mL/L~25mL/L,沙丁剂浓度0.2mL/L~1.0mL/L;其工艺条件为:温度30℃~50℃,pH值3.8~4.4,电压4V~10V,电流100A~500A,时间1500s~3000s;
更进一步地,水雾镍层的电镀液为硫酸镍浓度250g/L~300g/L,氯化镍浓度55g/L~60g/L,硼酸浓度25g/L~30g/L,镍S-A添加剂浓度15mL/L~25mL/L,镍S-B添加剂浓度15mL/L~25mL/L,沙丁剂浓度0.5mL/L~0.8mL/L;其工艺条件为:温度30℃~50℃,pH值3.8~4.4,电压4V~10V,电流100A~500A,时间1500s~3000s;
进一步地,步骤4中清洗过程依次为纯水清洗、超声波除油和纯水再次清洗。
进一步地,步骤5中PVD镀氮化锆层包括以下步骤:
将洁净水雾镍基片放入PVD炉体,并抽真空至5×10-4Pa,通入氩气,流量设定为150sccm~250sccm,调节腔体内工作压力至0.5Pa~1Pa,环境温度加热至100℃~120℃,将锆靶功率调整为20kW,预溅射900~1800s;预镀结束后,通入氮气,流量设定为20sccm~50sccm,维持炉体环境温度为120℃和腔体内工作压力为1Pa,转动基片台,转速为25rpm/min,打开锆靶的基片挡板,镀膜360s~1200s,关闭中频磁控溅射的电源,停止炉体内的氩气和氮气的通入。
另一方面,本发明还提供一种如上述方法制备得到的一种耐指纹哑金复合镀层。
本发明的积极效果如下:
1.本发明电镀铜时,所采用的铜层包括由打底铜层、焦磷酸铜层、硫酸铜层组成,这样的组合方式能保护基材,使得所可选择的基材更为广泛,不仅限于铜基或某一种基材。
究其原因为:打底铜能保护锌合金压铸件不受酸性镀液的腐蚀,并防止了置换镀,而使铜上的镀镍层具有较好的结合性,提高了合金压铸件镀层的抗蚀性能;焦磷酸铜具有分散性好、无毒、腐蚀性小以及均镀能力好的特点,能提高镀层的均匀性;硫酸铜具有优良的光亮与整平性能、分散性能和镀层韧性,容易抛光,耐腐蚀性极好等特点,能提高镀层光亮度,使镀层表面无麻点。
2.本发明电镀水雾镍层时,所采用的镍为水雾镍,水雾镍能使铜层表面有颗粒感,能呈现出哑光效果。
3.本发明PVD技术沉积形成ZrN钝化层时,相比PVD镀纯金,ZrN与底层材料的结合力更好,硬度也更高。
4.本发明所提供的耐指纹哑金镀层复合材料的制备方法,用电镀结合PVD技术,工艺简单、环保、生产周期短、成本低。
5.本发明所提供的耐指纹哑金镀层复合材料,铜层、镍层与氮化锆层,上述三层材料并不是单纯的叠加,而是互为铺垫,层层结合,最后制备得到的复合材料,哑金L值在75~85内,可控性强,具有非常好的耐指纹性能和高应力。
具体实施方式
下面结合实施例对本发明做进一步的描述,有必要在此指出的是以下实施例只是用于对本发明进行进一步的说明,不能理解为对本发明保护范围的限制,该领域的技术熟练人员根据上述发明内容所做出的一些非本质的改进和调整,仍属于本发明的保护范围。
实施例1
耐指纹哑金复合镀层的制备方法,包括以下步骤:
(1)电镀前处理:将金属基材表面清洗干净,进行镜面抛光处理和清洗处理;其中抛光处理包括开皮、研磨、整平和镜面精抛工艺;基材清洗处理分别通过超声波除蜡、超声波除油、电解和纯水清洗过程;
(2)电镀铜层:对步骤1处理后的洁净基材上,依次电镀打底铜层、焦磷酸铜层和硫酸铜层;
打底铜的电镀液为氰化亚铜浓度58g/L,游离氰化钠浓度20g/L;其工艺条件为:温度45℃,pH值12,电压4V,电流80A,时间1400s;
焦磷酸铜的电镀液为焦磷酸钾浓度350g/L,焦磷酸铜浓度45g/L,氨水浓度6mL/L,其工艺条件为:温度45℃,pH值8,电压4V,电流80A,时间1000s;
硫酸铜的电镀液为五水合硫酸铜浓度260g/L,硫酸浓度55g/L,其工艺条件为:温度35℃,pH值8,电压4V,电流280A,时间3500s;
(3)电镀水雾镍层:对步骤2制得的洁净硫酸铜层上电镀水雾镍层;
水雾镍层的电镀液为硫酸镍浓度280g/L,氯化镍浓度58g/L,硼酸浓度28g/L,镍S-A添加剂20mL/L,镍S-B添加剂20mL/L,沙丁剂0.6mL/L;其工艺条件为:温度40℃,pH值4,电压7V,电流300A,时间2500s;
(4)水雾镍基材清洗:对步骤3制得的水雾镍层,分别通过纯水清洗、超声波除油和再次纯水清洗;
(5)PVD镀氮化锆层:将步骤4制得的洁净水雾镍基片放入PVD炉体,并抽真空至5×10-4Pa,通入氩气,流量设定为200sccm,调节腔体内工作压力至1Pa,环境温度加热至120℃,将锆靶(中频磁控溅射)功率调整为20kW,预溅射1200s。预镀结束后,通入氮气,流量设定为35sccm,维持炉体环境温度为120℃和腔体内工作压力为1Pa,转动基片台,转速为25rpm/min,打开锆靶的基片挡板,镀膜720s,关闭中频磁控溅射的电源,停止炉体内的氩气和氮气的通入。
实施例2
耐指纹哑金复合镀层的制备方法,制备方法与实施例1基本相同,所不同的是,步骤5中氮气流量为40sccm。
实施例3
耐指纹哑金复合镀层的制备方法,制备方法与实施例1基本相同,所不同的是,步骤5中氮气流量为45sccm。
对比例1
电镀铜层后只电镀金层;即在实施例1的步骤1和步骤2基础上直接电镀金层。
金层的电镀液为氰化金钾浓度4g/L、JX-316A开缸液浓度600mL/L、JX-316B光亮剂20mL/L、JX-316C导盐浓度5mL/L、JX-316C导盐5mL/L;其工艺条件为:温度60℃,pH值5.5,电流密度0.6A/dm2,电镀时间10min。
对比例2
电镀铜层后只PVD镀氮化锆层,即在实施例1的步骤1和步骤2基础上直接进行步骤5PVD镀氮化锆层。
实施例4
对实施例1~3和对比例1~2,进行CASS盐雾测试(执行标准:ASTM B368)、耐指纹测试(用手直接接触样品)、附着强度试验测试(执行标准:GBT5270-2005)、外观(Lab值,执行标准:GB/T 17934.1-1999),所得的结果见表1。
表1
由上表1的数据可知:
1.实施例1~3比较,在进行PVD法镀氮化锆层时,预镀结束后,当氮气流量在35sccm~45sccm内,所制备得到的镀金复合材料,CASS盐雾测试12小时,都在10级范围内,都能耐指纹,都没有出现裂痕、剥离和起泡现象,哑金L值75~85范围内。
2.实施例与对比例1比较,当只采用电镀金层时,CASS盐雾测试12小时,在10级范围内,没有出现裂痕、剥离和起泡现象,但是有明显指纹,且哑金L值85~95之间。另外,直接电镀金层污染非常强,对生产人员健康形成威胁。
3.实施例与对比例2比较,当只采用PVD镀金层时,CASS盐雾测试12小时,在10级范围内,但是有明显指纹,镀层出现了剥离现象,且哑金L值85~95之间。
因此,本发明提供的一种耐指纹哑光复合材料制备方法具有非常很大的优势和应用价值。
Claims (9)
1.一种耐指纹哑金复合镀层的制备方法,其特征在于,包括步骤如下:
(1)将金属基材表面清洗干净,进行电镀前处理,包括镜面抛光处理和清洗处理;
(2)在步骤1处理后的洁净基材上电镀铜层,包括依次电镀打底铜层、焦磷酸铜层和硫酸铜层;
(3)在步骤2制得的洁净硫酸铜层上电镀水雾镍层;
(4)对步骤3制得的水雾镍层进行清洗;
(5)在步骤4处理后的洁净水雾镍层上PVD镀氮化锆层。
2.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤1中抛光处理包括开皮、研磨、整平和镜面精抛工艺;基材清洗处理分别通过超声波除蜡、超声波除油、电解和纯水清洗过程。
3.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤2中打底铜的电镀液为氰化亚铜浓度50g/L~65g/L,游离氰化钠浓度17g/L~25g/L;其工艺条件为:温度30℃~60℃,pH值11.5~13,电压2V~5V,电流50A~150A,时间1200s~1800s;
优选地,所述打底铜的电镀液为氰化亚铜浓度55g/L~60g/L,游离氰化钠浓度18g/L~22g/L;其工艺条件为:温度30℃~60℃,pH值11.5~13,电压2V~5V,电流50A~100A,时间1200s~1500s;
4.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤2中焦磷酸铜的电镀液为焦磷酸钾浓度300g/L~400g/L,焦磷酸铜浓度40g/L~50g/L,氨水浓度5mL/L~7mL/L,其工艺条件为:温度40℃~50℃,pH值7~9,电压1.5V~5V,电流50A~100A,时间800s~1500s;
优选地,所述焦磷酸铜的电镀液为焦磷酸钾浓度320g/L~380g/L,焦磷酸铜浓度40g/L~45g/L,氨水浓度5mL/L~7mL/L,其工艺条件为:温度40℃~50℃,pH值7~9,电压2V~4V,电流50A~100A,时间800s~1200s;
5.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤2中硫酸铜的电镀液为五水合硫酸铜浓度250g/L~300g/L,硫酸浓度50g/L~60g/L,其工艺条件为:温度30℃~50℃,pH值7~9,电压2V~6V,电流200A~400A,时间3000s~6000s;
优选地,所述硫酸铜的电镀液为五水合硫酸铜浓度250g/L~280g/L,硫酸浓度50g/L~60g/L,其工艺条件为:温度35℃~40℃,pH值7~9,电压2V~6V,电流250A~300A,时间3000s~4500s;
6.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤3中水雾镍层的电镀液为硫酸镍浓度200g/L~400g/L,氯化镍浓度50g/L~70g/L,硼酸浓度25g/L~35g/L,镍S-A添加剂浓度15mL/L~25mL/L,镍S-B添加剂浓度15mL/L~25mL/L,沙丁剂浓度0.2mL/L~1.0mL/L;其工艺条件为:温度30℃~50℃,pH值3.8~4.4,电压4V~10V,电流100A~500A,时间1500s~3000s;
优选地,所述水雾镍层的电镀液为硫酸镍浓度250g/L~300g/L,氯化镍浓度55g/L~60g/L,硼酸浓度25g/L~30g/L,镍S-A添加剂浓度15mL/L~25mL/L,镍S-B添加剂浓度15mL/L~25mL/L,沙丁剂浓度0.5mL/L~0.8mL/L;其工艺条件为:温度30℃~50℃,pH值3.8~4.4,电压4V~10V,电流100A~500A,时间1500s~3000s;
7.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤4中清洗过程依次为纯水清洗、超声波除油和纯水再次清洗。
8.如权利要求1所述的一种耐指纹哑金复合镀层的制备方法,其特征在于,所述步骤5中PVD镀氮化锆层包括以下步骤:
将洁净水雾镍基片放入PVD炉体,并抽真空至5×10-4Pa,通入氩气,流量设定为150sccm~250sccm,调节腔体内工作压力至0.5Pa~1Pa,环境温度加热至100℃~120℃,将锆靶功率调整为20kW,预溅射900~1800s;预镀结束后,通入氮气,流量设定为20sccm~50sccm,维持炉体环境温度为120℃和腔体内工作压力为1Pa,转动基片台,转速为25rpm/min,打开锆靶的基片挡板,镀膜360s~1200s,关闭中频磁控溅射的电源,停止炉体内的氩气和氮气的通入。
9.一种耐指纹哑金复合镀层,其特征在于,所述耐指纹哑金复合镀层由权利要求1至8任意一项所述的制备方法制备而得。
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