CN1463225A - 含有聚合物基础涂层的涂敷制品 - Google Patents

含有聚合物基础涂层的涂敷制品 Download PDF

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CN1463225A
CN1463225A CN02802045A CN02802045A CN1463225A CN 1463225 A CN1463225 A CN 1463225A CN 02802045 A CN02802045 A CN 02802045A CN 02802045 A CN02802045 A CN 02802045A CN 1463225 A CN1463225 A CN 1463225A
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refractory metal
layer
goods
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P·B·乔特
J·S·利普
陈国存
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Masco Corp
Masco Corp of Indiana
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Abstract

采用具有改进耐化学品性能和耐氧化性能的多层涂层涂敷制品。涂层包括在制品表面上的聚合物层，在聚合物层上的耐火金属或耐火金属合金触击层，和包含耐火金属氧化物或耐火金属合金氧化物的保护层。

Description

含有聚合物基础涂层的涂敷制品
发明领域
本发明涉及采用具有改进耐化学品性能和耐氧化性能的多层涂层涂敷的制品。
发明背景
目前对于各种黄铜制品如龙头、龙头罩、门旋钮、门把手、门锁眼盖等的实际情况是首先擦亮和抛光制品的表面到高光泽和然后涂敷保护性有机涂层(如由丙烯酸类、聚氨酯类、环氧类等组成的涂层)到此抛光的表面上。此体系的缺点是擦亮和抛光操作的劳动强度较大，特别是如果制品具有复杂的形状。同样，已知有机涂层并不总是如所需耐用的，和易于受酸的侵蚀。因此，如下情况是相当有利的：如果黄铜制品，或事实上其它制品，塑料、陶瓷、或金属，可以含有提供制品装饰性外观以及提供耐磨性，抗磨性和耐腐蚀性的涂层。在本领域已知的是可以将多层涂层涂敷到制品上，它提供装饰性外观以及提供耐磨性，抗磨性和耐腐蚀性。此多层涂层包括由耐火金属氮化物如氮化锆或氮化钛组成的装饰和保护性颜色层。此颜色层，当它是氮化锆时，提供黄铜颜色，和当它是氮化钛是提供金色。
U.S.专利Nos.5,922,478，6,033,790和5,654,108尤其描述了这样的涂层，它提供具有装饰性颜色的制品，如抛光的黄铜，且也提供耐磨性，抗磨性和耐腐蚀性。如果可以提供这样的涂层是非常有利的，该涂层提供与包含氮化锆或氮化钛基本相同的性能，但不是黄铜色的或金色的和提供改进的耐化学品性能和耐氧化性能。本发明提供这样的涂层。
发明概述
本发明涉及含有沉积在制品的至少一部分表面上的保护性多层涂层的制品如塑料、陶瓷或金属制品。更特别地，本发明涉及含有沉积在其表面上某些具体类型材料的多个重叠层的制品或基材，特别是金属制品如铝、黄铜或锌。涂层提供耐腐蚀性，耐磨性和抗磨性，和改进的耐化学品性能和耐氧化性能。
制品首先在它的表面上沉积有聚合物基础涂层。然后在聚合物基础涂层的顶部，通过气相沉积如物理气相沉积或化学气相沉积，沉积一个或多个气相沉积层。更特别地，直接沉积在基材表面上的第一层由聚合物材料组成。位于聚合物层上的是由耐火金属氧化物组成的保护层。
附图简述
图1是基材一部分不按比例的横截面图，基材含有在其上的聚合物基础涂层和在聚合物层上的保护层；
图2是相似于图1的视图，区别在于耐火金属或耐火金属合金触击层(strike layer)在聚合物层和保护层中间；和
图3是相似于图2的视图，区别在于耐火金属氧氮化物或耐火金属合金氧氮化物在该保护层上。
优选实施方案的描述
制品或基材12可以由如下物质组成：可以在其上涂敷镀敷层的任何材料，如塑料，如ABS、聚烯烃、聚氯乙烯、和酚醛树脂，陶瓷，金属或金属合金。在一个实施方案中，它由金属或金属合金如铜、钢、黄铜、锌、铝、镍合金等组成。
在本发明中，如图1-3所示，将聚合物或树脂基础涂层13涂敷到制品表面上。在聚合物层13上通过气相沉积涂敷耐火金属氧化物或耐火金属合金氧化物保护层32。聚合物层尤其用作平滑和覆盖制品表面中任何划痕或缺陷的基础涂层。聚合物基础涂层13可以由热塑性和热固性聚合物或树脂材料两者组成。这些聚合物或树脂材料包括公知的、常规和可购得的聚碳酸酯、环氧聚氨酯、聚丙烯酸酯、聚甲基丙烯酸酯、尼龙、聚酯、聚丙烯、聚环氧化物、醇酸树脂和含苯乙烯聚合物如聚苯乙烯、苯乙烯-丙烯腈(SAN)、苯乙烯-丁二烯、丙烯腈-丁二烯-苯乙烯(ABS)、及其共混物和共聚物。
聚碳酸酯描述在U.S.专利Nos.4,579,910和4,513,037，这两个文献在此引入作为参考。
尼龙和聚酰胺可以通过二胺和二羧酸的反应制备。通常用于制备尼龙的二胺和二羧酸一般包含2-约12个碳原子。尼龙也可通过另外的聚合制备。它们描述在“聚酰胺树脂”中，D.E.Floyd，ReinholdPublishing Corp.，纽约，1958，该文献在此引入作为参考。
聚环氧化物描述在H.Lee和K.Nevill的“环氧树脂”中，McGraw-Hill，纽约，1957，和描述在U.S.专利Nos.2,633,458、4,988,572、4,680,076、4,933,429和4,999,388中，所有这些文献在此引入作为参考。
聚酯是芳族二羧酸和二元醇的缩聚产物。芳族二羧酸包括对苯二甲酸、间苯二甲酸、4，4’-二苯基二羧酸、2，6-萘二羧酸等。二元醇包括含有2-约10个碳原子的低级链烷二醇，例如，乙二醇、丙二醇、环己烷二甲醇等。聚酯的一些说明性的非限制性例子包括聚对苯二甲酸乙二醇酯、聚苯二甲酸丁二醇酯、聚间苯二甲酸乙二醇酯、和聚(对苯二甲酸1，4-环己烷二甲醇酯)。它们公开于U.S.专利Nos.1,465,319、2,901,466和3,047,539中，所有文献在此引入作为参考。
聚丙烯酸酯和聚甲基丙烯酸酯是来自如下物质聚合的聚合物或树脂：一种或多种丙烯酸酯例如，丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯等；以及甲基丙烯酸酯，例如，甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、甲基丙烯酸己酯等。以上丙烯酸酯和甲基丙烯酸酯单体的共聚物也包括在当它出现于其中时的术语“聚丙烯酸酯”和“聚甲基丙烯酸酯”中。以提供用于本发明实施的聚丙烯酸酯树脂的单体丙烯酸酯和甲基丙烯酸酯的聚合可以通过任何公知的聚合技术完成。
苯乙烯-丙烯腈和丙烯腈-丁二烯-苯乙烯树脂和它们的制备，尤其公开于U.S.专利Nos.2,769,804、2,989,517、2,739,142、3,991,136、4,387,179中，所有这些文献在此引入作为参考。
醇酸树脂公开于“醇酸树脂技术”中，Patton，IntersciencePublishers，NY，NY，1962，和公开于U.S.专利Nos.3,102,866、3,228,787和4,511,692，所有这些文献在此引入作为参考。
环氧聚氨酯和它们的制备尤其公开于U.S.专利Nos.3,963,663、4,705,841、4,035,274、4,052,280、4,066,523、4,159,233、4,163,809、4,229,335和3,970,535,所有这些文献在此引入作为参考。特别有用的环氧聚氨酯是电涂在制品上的那些。这样的可电沉积环氧聚氨酯描述在上述U.S.专利Nos.3,963,663、4,066,523、4,159,233、4,035,274和4,070,258。
这些聚合物材料可非必要地包含常规和公知的填料如云母、滑石和玻璃纤维。
可以将聚合物基础涂层13涂敷到基材表面上，以尤其用于覆盖制品表面中任何划痕或缺陷和提供平滑和均匀的表面用于继续层如气相沉积层的沉积。
聚合物基础涂层13的厚度至少有效使制品或基材的表面变平。一般情况下，此厚度至少为为约0.12μm，优选至少约2.5μm，和更优选至少约5μm。上限厚度范围应当不超过约250μm。
在一些情况下，依赖于基材材料和聚合物基础涂层的类型，聚合物基础涂层并不充分粘合到基材上。在这样的状况下，在基材上沉积底漆层以改进聚合物基础涂层对基材的粘合。底漆层可以尤其由卤化聚烯烃组成。卤化聚烯烃是一般可市售的常规和公知的聚合物。优选的卤化聚烯烃是氟化和溴化聚烯烃，更优选是氯化聚烯烃。卤化聚烯烃，特别是氯化聚烯烃和它们的制备方法一起尤其公开于U.S.专利Nos.5,319,032、5,840,783、5,385,979、5,198,485、5,863,646、5,489,650和4,273,894，所有这些文献在此引入作为参考。
底漆层的厚度是有效改进聚合物基础涂层对基材粘合的厚度。一般情况下此厚度至少为约0.25μm。上限厚度不是关键的和一般由次要的如成本和外观的考虑来控制。一般情况下应当不超过约125μm的上限厚度。
如图1所示，在聚合物层上，通过气相沉积如物理气相沉积或化学气相沉积，沉积由耐火金属氧化物或耐火金属合金氧化物组成的保护和装饰性层32。
构成耐火金属氧化物的耐火金属是锆、钛、铪等，优选锆、钛或铪。耐火金属合金如锆-钛合金、锆-铪合金、钛-铪合金等也可用于形成氧化物。因此，例如，氧化物可包括锆-钛合金氧化物。
此保护层32的厚度是至少有效提供抗磨性，耐擦划性，耐磨性，和改进的耐化学品性能和耐氧化性能的厚度。一般情况下，此厚度至少为约1,000埃，优选至少约1,500埃，和更优选至少约2,500埃。厚度上限范围一般不是关键的且依赖于次要的考虑如成本。一般情况下不应当超过约0.75μm，优选约0.5μm的厚度。
沉积层32的一种方法是通过采用反应溅射或反应阴极弧蒸发的物理气相沉积。反应阴极弧蒸发和反应溅射一般相似于通常溅射和阴极弧蒸发，区别在于将反应性气体引入腔室中，它与移除的目标材料反应。因此，在其中层32由氧化锆组成的此情况下，阴极由锆组成，和氧气是引入腔室的反应性气体。
除保护层32以外涂层可包含其它气相沉积层。如图2和3所示，耐火金属或耐火金属合金触击层31位于保护层32和聚合物层中间。层31的厚度一般至少有效使层31用作触击层。一般情况下，此厚度至少为约60埃，优选至少约120埃，和更优选至少约250埃。上限厚度范围不是关键的且一般依赖于如成本的考虑。然而，一般情况下，层31应当不厚于约1.2μm，优选约0.5μm，和更优选约0.25μm。
通过常规和公知的气相沉积技术包括物理气相沉积技术如阴极弧蒸发(CAE)或溅射，沉积耐火金属或耐火金属合金层31。溅射技术和设备，尤其描述于J.Vossen和W.Kern“薄膜工艺II”，Academic Press，1991；R.Boxman等人，“真空弧科学和技术手册”，Noyes Pub.，1995；和U.S.专利Nos.4,162,954和4,591,418，所有这些文献在此引入作为参考。
简单地，在溅射沉积工艺中，将耐火金属(如钛或锆)目标(它是阴极)和基材放入真空腔室中。将腔室中的空气抽空以在腔室中产生真空条件。将惰性气体，如氩气，引入腔室。将气体粒子电离和向目标加速以移除钛或锆原子。然后将移除的目标材料典型地作为涂料膜沉积在基材上。
在阴极弧蒸发中，将典型地几百安培的电弧撞击在金属阴极如锆或钛的表面。弧蒸发阴极材料，它然后冷凝在基材上，形成涂层。
在本发明的优选实施方案中，耐火金属由钛或锆，优选锆组成，和耐火金属合金由锆-钛合金组成。
如图3所示，在保护层32上可以是由耐火金属或耐火金属合金，氧气和氮气反应产物组成的薄层34。耐火金属或耐火金属合金，氧气和氮气的反应产物一般由耐火金属氧化物或耐火金属合金氧化物，耐火金属氮化物或耐火金属合金氮化物，和耐火金属氧氮化物或耐火金属合金氧氮化物组成。因此，例如锆、氧气和氮气的反应产物包括氧化锆、氮化锆和氧氮化锆。包括氧化锆和氮化锆合金的这些耐火金属氧化物和耐火金属氮化物和它们的制备和沉积是常规的和公知的，且尤其描述于U.S.专利No.5,367,285，该文献的公开内容在此引入作为参考。
层34有效提供对涂层的另外改进的耐氧化性能和耐化学品，如酸或碱性能。层34通常具有至少有效提供另外改进的耐氧化性能和耐化学品性能的厚度。一般情况下层34的厚度至少为约10埃，优选至少约25埃，和更优选至少约40埃。一般情况下层34应当不厚于约0.10μm，优选约250埃，和更优选约100埃。
为更容易理解本发明，提供以下实施例。实施例是说明性和并不将本发明限定于此。
实施例
将黄铜龙头放入包含标准和公知的肥皂，洗涤剂，抗絮凝剂等的常规浸泡清洁剂浴中，将该浴保持在8.9-9.2的pH和180-200°F的温度下约10分钟。
将龙头浸入阴极电沉积浴中，阴极电沉积浴包含从LillyIndustries以商品名Micro Finish购得的多元胺和环氧聚氨酯的反应产物。树脂由Lilly Industries以大约25-40％固体下提供且由去离子水稀释到3％-20％的固体范围。通过施加约50-400D.C.伏约3分钟在阴极基材(龙头)上沉积聚合物基础涂层，电沉积浴温度为约75°F-120°F。将聚合物涂敷的龙头从电沉积浴取出和采用水清洗。将聚合物涂敷的龙头放入烘箱和将聚合物在约300°F下固化约18分钟，随后在约500°F-约560°F下再固化18分钟。获得的聚合物基础涂层厚度为约0.5密耳。
将聚合物涂敷的龙头放入阴极弧蒸发镀敷容器中。容器一般是包含真空腔室的圆筒形外壳，真空腔适于通过泵抽空。通过用于改变进入腔室氩气流量的可调节阀门，将氩气源连接到腔室。此外，通过用于改变进入腔室氧气流量的可调节阀门，将氧气源连接到腔室。
将圆筒形阴极安装在腔室中心和连接到可变D.C.电源的负输出上。将电源的正侧连接到腔室壁上。阴极材料包括锆。
将聚合物涂敷的龙头安装在转轴上，将16个这样的转轴安装在围绕阴极外部的环上。整个环围绕阴极旋转而每个转轴也围绕它自身的轴旋转，导致所谓的行星运动，它对于围绕每个转轴安装的多个龙头提供对阴极的均匀曝露。环典型地以几个rpm旋转，而每个转轴相对于每个环回转进行几个回转。转轴与腔室电隔离且设置有可旋转接触使得可以在涂敷期间将偏压施加到基材上。
将真空腔室抽空到约5×10-3毫巴的压力和加热到约100℃。
然后对涂敷的龙头进行高偏压弧等离子体清洁，其中将约500伏的(负)偏压施加到涂敷的龙头上同时将大约500安培的弧撞击和保持在阴极上。清洁的持续时间大约是5分钟。
在足以保持约1-5毫托压力的速率下引入氩气。在3分钟时间期间内，在聚合物基础涂层涂敷的龙头上沉积平均厚度为约0.1μm的锆层。阴极弧沉积工艺包括施加D.C.电源到阴极上以达到约460安培的电流，向容器中引入氩气以保持容器中压力在约2毫托下且以上述行星方式旋转龙头。
在沉积锆层之后，在锆层上沉积由氧化锆组成的保护层。在约250sccm下持续氩气的流量和在约375sccm的流量下引入氧气，而弧放电在大约460安培下持续。氩气和氧气的流动持续约40分钟。保护层的厚度为约3500-4500埃。在沉积此保护层之后，将弧熄灭，将真空腔室排气和取出涂敷制品。
尽管已经为了说明的目的描述了本发明的某些实施方案，理解在本发明一般范围中可以有各种实施方案和改进。

Claims (9)

1.一种在其至少一部分表面上含有多层涂层的制品，包括：
聚合物层；
由耐火金属氧化物或耐火金属合金氧化物组成的保护层。
2.权利要求1的制品，其中由耐火金属或耐火金属合金组成的触击层在该聚合物层和该保护层中间。
3.权利要求2的制品，其中由耐火金属或耐火金属合金，氧气和氮气反应产物组成的层在该保护层上。
4.权利要求1的制品，其中由耐火金属或耐火金属合金，氧气和氮气反应产物组成的层在该保护层上。
5.权利要求1的制品，其中该聚合物层由环氧聚氨酯组成。
6.一种在其至少一部分表面上含有具有改进耐化学品性能和耐氧化性能的多层涂层的制品，包括：
在该制品表面上的聚合物层；和
由耐火金属氧化物或耐火金属合金氧化物组成的保护层。
7.权利要求6的制品，其中由耐火金属或耐火金属合金组成的层在该聚合物层和该保护层中间。
8.权利要求7的制品，其中该聚合物层由环氧聚氨酯组成。
9.权利要求6的制品，其中由耐火金属或耐火金属合金，氧气和氮气反应产物组成的层在该保护层上。
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