CN102108484B - 一种双层抗菌镀层的制备方法 - Google Patents
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Abstract
一种双层抗菌镀层的制备方法,涉及一种塑胶制品金属化。将塑胶基材放入物理气相沉积真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化,得活化后的基材;对活化后的基材表面真空镀金属底膜;对已镀金属底膜的基材喷镀抗菌中间涂层;对喷完中间抗菌层的样品进行物理气相沉积镀抗菌金属膜,得双层抗菌镀层。具有双层抗菌层,利用PVD真空镀的膜层不致密,存在大量微孔,中间抗菌层的抗菌剂可通过这些空洞迁移到镀层表面与表面抗菌镀层一起对细菌进行杀死或者抑制其生长。适用于卫浴、电子、家电与汽车等行业。
Description
技术领域
本发明涉及一种塑胶制品金属化,尤其是涉及一种新型双层抗菌镀层的制备方法。
背景技术
进入21世纪以来,塑料制品已成为人们的日常生活中必不可少的一部分,其广泛应用于我们生活的每一个细节,例如在人们日常接触的各种家用电器(电话、洗衣机、电脑、电器开关等)当中已经大量采用了塑料制品。另一方面由于环境污染等原因的影响,这些人们日常接触的这些塑料制品的表面往往会带有大量的细菌,成为一个个细菌污染源和疾病传播源。据统计,全世界每年死亡人数中大约有1700万人是因细菌传染而引起的。那么发展和研究具有抗菌性能的新型镀层制品,对于改善人们的生活环境、减少疾病发生率、保护人类身体健康等方面都具有十分重要的现实意义。
从2003年SARS病毒全球泛滥到最近H1N1流感的全球性爆发,让消费者对食品安全和环境中存在各种病原菌的担心加剧。全球抗菌剂在塑料中应用日益广泛,以满足人们对公共卫生和日常生活需求,全球抗菌剂在塑料中应用的年增长率约为3.5%~4%。北美是使用抗菌剂(包括生物抑制剂)最多的地区,占全球总用量的40%,日本占20%。而日本的人均抗菌剂使用量最大,远超北美和欧洲。根据世界知名的民意调查公司Gallup poll最近发布的一项调查显示,绝大多数的消费者表示愿意购买有抗菌保护的抗菌产品,75%的消费者偏爱选择具有抗菌保护的产品。调查里10人有7人以上透露有用到超过6样抗菌产品。消费者感觉在用途和环境方面有必要使用抗菌加工的制品。
中国专利ZL200420071581公开一种表面抗菌耐磨制品,其基材是金属制品、无机材料制品、高分子材料制品,通过物理气相沉积技术在上述基材表面上镀含有银或铜或银铜复合物的硬质膜。该发明的镀层的耐磨性不够好,抗菌性持续效果差。
发明内容
本发明的目的在于针对现有技术的上述不足,提供一种具有长期抗菌和抑菌效果的双层抗菌镀层的制备方法。
本发明包括以下步骤:
1)将塑胶基材放入物理气相沉积(PVD)真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化,得活化后的基材;
在步骤1)中,所述塑胶基材可选自热塑性塑胶或热固性塑胶等,所述热塑性塑胶可选自ABS、PC/ABS、HIPS、PC、PPO、PP、PERT、HDPE、PA6、PA66、ABS/TPU、玻纤增强PA6、玻纤增强PP等中的一种;所述热固性塑胶可采用BMC等;所述活化,可采用等离子辉光活化,其工艺条件可为离子源电流0.3~0.5A,偏压80~150V,占空比50%~80%,氩气流速10~100SCCM,氧气流速10~150SCCM,炉内真空压力0.1~0.3Pa,活化时间5~10min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
2)对活化后的基材表面真空镀金属底膜;
在步骤2)中,所述对基材表面真空镀金属底膜,可采用中频溅射法,所述中频溅射法的工艺条件如下:中频电源功率6~9kW,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间10~20min;所述金属底膜可选自Cu,Cr,Cu-Zn合金等中的至少一种。
3)对已镀金属底膜的基材喷镀抗菌中间涂层;
在步骤3)中,所述抗菌中间涂层可为添加有机抗菌剂或无机抗菌剂的紫外光固化油漆、烤漆、电泳漆、静电粉末漆等中的至少一种;所述紫外光固化油漆可采用UV漆等;所述有机抗菌剂可选自二氯十辛基异噻唑啉酮(Dichlorooctylisothiazolinone,DCOIT)、3-(三甲氧甲硅烷基)丙基十八烷基二甲基氯化铵,DC5700、10,10’-氧代双吩恶砒(OBPA)、磷酸酯复合物、PolySept L型抗菌剂等中的至少一种;所述二氯十辛基异噻唑啉酮(Dichlorooctylisothiazolinone,DCOIT)可选自罗门哈斯公司vinyzene的二氯十辛基异噻唑啉酮(Dichlorooctylisothiazolinone,DCOIT);所述3-(三甲氧甲硅烷基)丙基十八烷基二甲基氯化铵可选自美国道康宁公司的3-(三甲氧甲硅烷基)丙基十八烷基二甲基氯化铵;所述10,10’-氧代双吩恶砒(OBPA)可选自托洛伊公司(Troy Corporation)的10,10’-氧代双吩恶砒(OBPA);所述磷酸酯复合物可选自聚合化学合金公司(PolyChem Alloy)的磷酸酯复合物;所述无机抗菌剂可选自纳米银、纳米铜等中的至少一种;所述对已镀金属底膜的基材喷镀抗菌中间涂层的具体方法可为:在塑胶基体上喷镀一层添加1%~10%抗菌剂的漆层,再送入红外线烘炉,进行喷漆膜层流平、烘干,烘干后的喷漆膜层在紫外线光固化炉内接受照射固化交联,照射固化交联的时间可为10~45s;所述漆层的厚度可为10~30μm;所述烘干的温度可为50~70℃,烘干的时间可为3~10min;所述漆层可采用UV漆层,电泳漆层或粉末漆层等。
4)对喷完中间抗菌层的样品进行物理气相沉积镀抗菌金属膜,得双层抗菌镀层。
在步骤4)中,所述物理气相沉积镀抗菌金属膜可采用电弧法或中频溅射法等,所述电弧法的工艺条件可为:靶电源电流60~100A,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间1~5min;所述中频溅射法的工艺条件可为:中频电源功率6~9kW,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间5~10min;所述抗菌金属膜的靶材可为:Cr95%~99.5%Ag5%~0.5%合金靶材。
与现有技术相比,本发明具有以下突出优点:
1)具有双层抗菌层,利用PVD真空镀的膜层不致密,存在大量微孔,中间抗菌层的抗菌剂可通过这些空洞迁移到镀层表面与表面抗菌镀层一起对细菌进行杀死或者抑制其生长。
2)利用PVD真空镀的膜层不致密,存在大量的微孔,中间抗菌层的抗菌剂可通过这些空洞迁移到镀层的表面与表面抗菌镀层一起对细菌进行杀死或者抑制其生长,因此这种双层抗菌镀层不仅具有长期的抗菌和抑菌效果,而且抗菌和抑菌效率高。
3)此种金属膜/抗菌层/金属抗菌膜之双层抗菌技术开拓了广谱塑胶金属化领域,镀出产品功能优异且外观优良,非常适用于卫浴、电子、家电与汽车等行业。
附图说明
图1为本发明实施例1的PVD Cr99.5%Ag0.5%表面微孔分布图。在图1中,300×放大微孔数:2640pcs/cm2,微孔尺寸为8.3μm;计算微孔数量及微孔尺寸是在取边长为0.25mm的正方形中进行。
具体实施方式
实施例1
一种PC/ABS镜壳镀双层抗菌镀层示例,其工艺流程如下:
(1)将PC/ABS注塑成型坯件放入PVD真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化(等离子辉光),其工艺条件为离子源电流0.5A,偏压150V,占空比80%,氩气流速100SCCM,氧气流速150SCCM,炉内真空压力0.3Pa,活化时间10min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
(2)对将PC/ABS注塑成型坯件表面真空镀金属底膜,其工艺条件为中频溅射法工艺条件:中频电源功率9KW,偏压150V,氩气流速100SCCM,炉内真空压力0.3Pa,镀膜时间20min);所述的底层金属膜为纯Cu。
(3)对已镀PVD金属底层的样品喷镀抗菌中间涂层为添加无机抗菌剂的UV涂层其工艺包含以下程序,依次:
a.喷镀一层添加1%纳米银抗菌剂的UV漆层,漆层厚30μm。
b.塑胶件送入红外线烘炉,进行喷漆膜层流平、烘干(50℃×10min)。
c.流平后喷漆膜层在紫外线光固化炉内接受照射固化交联(时间45s)。
(4).对喷完中间抗菌层的样品进行PVD镀抗菌金属膜,其电弧法工艺条件:靶电源电流100A,偏压150V,氩气流速100SCCM,炉内真空压力0.3Pa,镀膜时间5min);所述的抗菌金属膜靶材为:Cr99.5%Ag0.5%合金靶材。PVD Cr99.5%Ag0.5%表面微孔分布图见图1。
样品依据JIS Z2801:2000 Antimicrobial-Test for antimicrobial activity and efficacy标准进行检测,检测结果如表1所示。
表1
实施例2
在玻纤增强PPO塑胶基材镀双层抗菌镀层应用示例,其工艺流程如下:
(1)将玻纤增强PPO塑胶基体放入PVD真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化(等离子辉光),其工艺条件为离子源电流0.3A,偏压80V,占空比50%,氩气流速10SCCM,氧气流速50SCCM,炉内真空压力0.1Pa,活化时间5min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
(2)对玻纤增强PPO塑胶基材表面真空镀金属底膜,其工艺条件为中频溅射法工艺条件:中频电源功率6kW,偏压80V,氩气流速20SCCM,炉内真空压力0.1Pa,镀膜时间10min);所述的底层金属膜为Cu-Zn合金。
(3)对已镀PVD金属底层的样品喷镀抗菌中间涂层为添加无机抗菌剂的UV涂层其工艺包含以下程序,依次:
a.喷镀一层添加10%纳米铜抗菌剂的UV漆层,漆层厚10μm。
b.塑胶件送入红外线烘炉,进行喷漆膜层流平、烘干(70℃×3min)。
c.流平后喷漆膜层在紫外线光固化炉内接受照射固化交联(时间10s)。
(4)对喷完中间抗菌层的样品进行PVD镀抗菌金属膜,中频溅射法工艺条件:中频电源功率9KW,偏压150V,氩气流速100SCCM,炉内真空压力0.3Pa,镀膜时间10min),所述的抗菌金属膜靶材为Cr5%Ag5%合金靶材。
实施例3
一种PA6加玻纤矿粉(增强型PA6)镀双层抗菌镀层水龙头示例,其工艺流程如下:
(1)将PA6加玻纤矿粉(增强型PA6)胶件基体放入PVD真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化(等离子辉光),其工艺条件为离子源电流0.4A,偏压100V,占空比70%,氩气流速50SCCM,氧气流速100SCCM,炉内真空压力0.2Pa,活化时间8min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
(2)对PA6加玻纤矿粉(增强型PA6)胶件基材表面真空镀金属底膜,其工艺条件为中频溅射法工艺条件:中频电源功率8KW,偏压120V,氩气流速70SCCM,炉内真空压力0.2Pa,镀膜时间15min);所述的底层金属膜为纯Cr。
(3)对已镀PVD金属底层的样品喷镀抗菌中间涂层为添加有机抗菌剂的UV。其工艺包含以下程序,依次:
a.喷镀一层添加3%罗门哈斯公司的DCOIT抗菌剂的UV漆层,漆层厚20μm。
b.塑胶件送入红外线烘炉,进行喷漆膜层流平、烘干(60℃×8min)。
c.流平后喷漆膜层在紫外线光固化炉内接受照射固化交联(时间30s)。
(4).对喷完中间抗菌层的样品进行PVD镀抗菌金属膜,其电弧法工艺条件:靶电源电流100A,偏压100V,氩气流速70SCCM,炉内真空压力0.2Pa,镀膜时间3min),所述的抗菌金属膜靶材为:Cr98%Ag2%合金靶材。
样品依据JIS Z2801:2000 Antimicrobial-Test for antimicrobial activity and efficacy标准进行检测,检测结果如表2所示。
表2
实施例4
一种BMC热固性塑胶坯件镀双层抗菌镀层冰箱把手示例,其工艺流程如下:
(1)将BMC热固性塑胶坯件基体放入PVD真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化(等离子辉光),其工艺条件为离子源电流0.5A,偏压120V,占空比60%,氩气流速100SCCM,氧气流速100SCCM,炉内真空压力0.2Pa,活化时间10min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
(2)对BMC热固性塑胶坯件基材表面真空镀金属底膜,其工艺条件为中频溅射法工艺条件:中频电源功率7KW,偏压100V,氩气流速30SCCM,炉内真空压力0.1Pa,镀膜时间10min);所述的底层金属膜为纯Cr。
(3)对已镀PVD金属底层的样品喷镀抗菌中间涂层为添加有机抗菌剂的UV。其工艺包含以下程序,依次:
a.喷镀一层添加6%托洛伊公司的10,10’-氧代双吩恶砒(OBPA)抗菌剂的UV漆,漆层厚约15μm。
b.塑胶件送入红外线烘炉,进行喷漆膜层流平、烘干(62℃×9min)。
c.流平后喷漆膜层在紫外线光固化炉内接受照射固化交联(时间25s)。
(4).对喷完中间抗菌层的样品进行PVD镀抗菌金属膜,其电弧法工艺条件:靶电源电流80A,偏压80V,氩气流速50SCCM,炉内真空压力0.15Pa,镀膜时间2min),所述的抗菌金属膜靶材为Cr97%Ag3%合金靶材。
实施例5
一种ABS镜框镀双层抗菌镀层生产示例,其工艺流程如下:
(1)将ABS镜框胶件基体放入PVD真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化(等离子辉光),其工艺条件为离子源电流0.3A,偏压120V,占空比60%,氩气流速80SCCM,氧气流速120SCCM,炉内真空压力0.2Pa,活化时间5min,以达到清洁及化活化基体表面之目的,提高抗菌除氯膜与基材间的结合力。
(2)对ABS镜框胶件基材表面真空镀金属底膜,其工艺条件为中频溅射法工艺条件:中频电源功率7kW,偏压100V,氩气流速70SCCM,炉内真空压力0.2Pa,镀膜时间20min);所述的底层金属膜为纯Cu。
(3)对已镀PVD金属底层的样品喷镀抗菌中间涂层为添加有机抗菌剂的UV。其工艺包含以下程序,依次:
a.喷镀一层添加10%聚合化学合金公司的“PolySept L”抗菌剂的UV漆层,漆层厚10μm。
b.塑胶件送入红外线烘炉,进行喷漆膜层流平、烘干(55℃×10min)。
c.流平后喷漆膜层在紫外线光固化炉内接受照射固化交联(时间10s)。
(4)喷完中间抗菌层的样品进行PVD镀抗菌金属膜,中频溅射法工艺条件:中频电源功率8kW,偏压100V,氩气流速20SCCM,炉内真空压力0.1Pa,镀膜时间10min),所述的抗菌金属膜靶材为Cr96%Ag4%合金靶材。
Claims (4)
1.一种双层抗菌镀层的制备方法,其特征在于以下步骤:
1)将塑胶基材放入物理气相沉积真空设备中,进行抽真空,当真空度达到10-2时,对基材实施清洗与活化,得活化后的基材;
2)对活化后的基材表面真空镀金属底膜;
3)对已镀金属底膜的基材喷镀抗菌中间涂层;所述抗菌中间涂层为添加有机抗菌剂或无机抗菌剂的紫外光固化油漆、电泳漆、静电粉末漆中的一种;所述有机抗菌剂选自二氯十辛基异噻唑啉酮、3-(三甲氧甲硅烷基)丙基十八烷基二甲基氯化铵,DC5700、10,10’-氧代双吩恶砒、磷酸酯复合物、PolySept L型抗菌剂中的一种;所述无机抗菌剂选自纳米银、纳米铜中的一种;所述紫外光固化油漆采用UV漆;所述对已镀金属底膜的基材喷镀抗菌中间涂层的具体方法为:在塑胶基体上喷镀一层添加1%~10%抗菌剂的漆层,再送入红外线烘炉,进行喷漆膜层流平、烘干,烘干后的喷漆膜层在紫外线光固化炉内接受照射固化交联,照射固化交联的时间为10~45s;所述漆层的厚度为10~30μm;所述烘干的温度为50~70℃,烘干的时间为3~10min;
4)对喷完中间抗菌层的样品进行物理气相沉积镀抗菌金属膜,得双层抗菌镀层;所述物理气相沉积镀抗菌金属膜是采用电弧法或中频溅射法;所述电弧法的工艺条件为:靶电源电流60~100A,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间1~5min;所述中频溅射法的工艺条件为:中频电源功率6~9kW,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间5~10min;所述抗菌金属膜的靶材为:Cr95%~99.5%Ag5%~0.5%合金靶材。
2.如权利要求1所述的一种双层抗菌镀层的制备方法,其特征在于在步骤1)中,所述塑胶基材选自热塑性塑胶或热固性塑胶,所述热塑性塑胶选自ABS、PC/ABS、HIPS、PC、PPO、PP、PERT、HDPE、PA6、PA66、ABS/TPU、玻纤增强PA6、玻纤增强PP中的一种;所述热固性塑胶采用BMC。
3.如权利要求1所述的一种双层抗菌镀层的制备方法,其特征在于在步骤1)中,所述活化,是采用等离子辉光活化,其工艺条件为离子源电流0.3~0.5A,偏压80~150V,占空比50%~80%,氩气流速10~100SCCM,氧气流速10~150SCCM,炉内真空压力0.1~0.3Pa,活化时间5~10min。
4.如权利要求1所述的一种双层抗菌镀层的制备方法,其特征在于在步骤2)中,所述对基材表面真空镀金属底膜,是采用中频溅射法,所述中频溅射法的工艺条件如下:中频电源功率6~9kW,偏压80~150V,氩气流速20~100SCCM,炉内真空压力0.1~0.3Pa,镀膜时间10~20min;所述金属底膜选自Cu,Cr,Cu-Zn合金中的至少一种。
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