CN102691039A - 抗菌镀膜件及其制备方法 - Google Patents

抗菌镀膜件及其制备方法 Download PDF

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CN102691039A
CN102691039A CN2011100730918A CN201110073091A CN102691039A CN 102691039 A CN102691039 A CN 102691039A CN 2011100730918 A CN2011100730918 A CN 2011100730918A CN 201110073091 A CN201110073091 A CN 201110073091A CN 102691039 A CN102691039 A CN 102691039A
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titanium
base material
antibiotic layer
coating
spare
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张新倍
陈文荣
蒋焕梧
陈正士
胡智杰
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Priority to TW100110978A priority patent/TW201239117A/zh
Priority to US13/210,752 priority patent/US20120244386A1/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/568—Transferring the substrates through a series of coating stations
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
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Abstract

本发明提供一种具有持久抗菌效果的抗菌镀膜件，其包括基材，形成于基材表面的抗菌层及形成于抗菌层表面的防氧化层，该抗菌层包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布。本发明抗菌镀膜件的抗菌层中的铜膜起抗菌作用，钛膜可起防氧化的作用，同时钛膜可缓释抗菌层中铜离子的溶出，使抗菌层具有长效的抗菌效果，相应延长抗菌镀膜件的使用寿命。此外，本发明还提供一种所述抗菌镀膜件的制备方法。

Description

抗菌镀膜件及其制备方法
技术领域
本发明涉及一种抗菌镀膜件及其制备方法。
背景技术
有害细菌的传播和感染严重威胁着人类的健康，尤其是近年来SARS病毒、禽流感等的传播和感染，使抗菌材料在日常生活中的应用迅速发展起来。目前常用的抗菌材料有两种，金属抗菌材料和光催化抗菌材料。
常见的金属抗菌材料为铜、锌及银等，它们的抗菌机理是﹕抗菌金属缓慢释放出金属离子如Cu2+、Zn2+，当微量的具有杀菌性的金属离子与细菌等微生物接触时，该金属离子依靠库伦力与带有负电荷的微生物牢固吸附，金属离子穿透细胞壁与细菌体内蛋白质上的巯基、氨基发生反应，使蛋白质活性破坏，使细胞丧失***增殖能力而死亡，从而达到杀菌的目的。使用过程中，随着金属离子的消耗流失，金属抗菌材料的杀菌效果会逐渐减低；且金属抗菌材料的表面容易氧化变色，影响材料的整体抗菌效果。
发明内容
有鉴于此，有必要提供一种抗菌效果较为持久的抗菌镀膜件。
另外，还有必要提供一种上述抗菌镀膜件的制备方法。
一种抗菌镀膜件，其包括基材，形成于基材表面的抗菌层及形成于抗菌层表面的防氧化层，该抗菌层包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布。
一种抗菌镀膜件的制备方法，其包括如下步骤：
提供基材；
在该基材的表面形成抗菌层，该抗菌层包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布；
在该抗菌层的表面形成防氧化层。
本发明所述抗菌镀膜件的抗菌层为铜膜和钛膜的交替多层膜，所述抗菌层中铜膜起抗菌作用，钛膜可起防氧化的作用，同时钛膜可缓释抗菌层中铜离子的溶出，使抗菌层具有长效的抗菌效果，相应延长抗菌镀膜件的使用寿命。
附图说明
图1为本发明一较佳实施例的抗菌镀膜件的剖视图；
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
抗菌镀膜件 10
基材 11
打底层 13
抗菌层 15
防氧化层 17
真空镀膜机 20
镀膜室 21
钛靶 23
铜靶 24
轨迹 25
真空泵 30
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，本发明一较佳实施方式的抗菌镀膜件10包括基材11、形成于基材11表面的打底层13、形成于打底层13表面的抗菌层15及形成于抗菌层15表面的防氧化层17。
该基材11的材质优选为不锈钢，但不限于不锈钢。
该打底层13可以磁控溅射的方式形成。该打底层13为金属钛层。该打底层13的厚度为50～100nm。
该抗菌层15可以磁控溅射的方式形成。所述抗菌层15包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布。所述抗菌层15的厚度为0.7～1.5μm。所述抗菌层15中铜膜起抗菌作用，钛膜可起防氧化的作用，同时钛膜可缓释抗菌层15中金属铜离子的溶出，使抗菌层15具有长效的抗菌效果。抗菌层15与所述打底层13直接结合的可为铜膜或钛膜。
该防氧化层17可以磁控溅射的方式形成。该防氧化层17为金属钛层，其可保护抗菌层15避免其氧化。该防氧化层17的厚度为20～100nm。抗菌层15与所述防氧化层17直接结合的可为铜膜或钛膜。
本发明一较佳实施方式的抗菌镀膜件10的制备方法，其包括如下步骤：
提供基材11，该基材11的材质优选为不锈钢，但不限于不锈钢。
对该基材11进行预处理。该预处理包括常规的除油、除蜡、酸洗、中和、去离子水清洗、烘干等步骤。
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)、相对设置的二钛靶23和相对设置的二铜靶24。镀膜时，转架带动基材11沿圆形的轨迹25公转，且基材11在沿轨迹25公转时亦自转；当基材11转到钛靶23处时，基材11的一表面将被沉积钛原子；当基材11转到铜靶24处时，基材11的一表面将被沉积铜原子，如此基材11围绕轨迹25转动一圈，基材11表面将被沉积一钛膜和一铜膜。
采用磁控溅射法在经预处理的基材11的表面溅镀打底层13，该打底层13为一金属钛层。溅镀该打底层13在所述真空镀膜机20中进行，使用钛靶23。溅镀时，开启钛靶23，设置钛靶23的功率为5～10kw，通入工作气体氩气，氩气流量为100～300sccm，对基材11施加-50～-250V的偏压，镀膜温度为50～250℃，镀膜时间为5～10min。该打底层13的厚度为50～100nm。
继续采用磁控溅射法在所述打底层13的表面溅镀抗菌层15，该抗菌层15为铜膜和钛膜的交替多层膜。继续开启钛靶23，设置钛靶23的功率为5～10kw，同时开启铜靶24，设置铜靶24的功率为2～8kw，通入工作气体氩气，氩气流量为100～300sccm，对基材11施加偏压大小为-50～-250V，镀膜温度为50～250℃，镀膜时间为10～30min。该抗菌层15的厚度为0.7～1.5μm。
继续采用磁控溅射法在所述抗菌层15的表面溅镀防氧化层17。继续开启钛靶23，保持钛靶23的功率为5～10kw，同时关闭铜靶24，通入工作气体氩气，氩气流量为100～300sccm，对基材11施加偏压大小为-50～-250V，镀膜温度为50～250℃，镀膜时间为1～10min。该防氧化层17的厚度为20～100nm。
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为磁控溅射镀膜机。
本实施例所使用的基材11的材质为不锈钢。
溅镀打底层13：钛靶23的功率为8kw，氩气流量为150sccm，基材11的偏压为-50V，镀膜温度为120℃，镀膜时间为10min；该打底层13的厚度为100nm；
溅镀抗菌层15：钛靶23的功率为8kw，铜靶24的功率为8kw，氩气流量为150sccm，基材11的偏压为-50V，镀膜温度为120℃，镀膜时间为15min；该抗菌层15的厚度为900nm。
溅镀防氧化层17：钛靶23的功率为8kw，基材11的偏压为-50V，氩气流量为150sccm，镀膜温度为120℃，镀膜时间为5min；该防氧化层17的厚度为50nm。
实施例2
本实施例所使用的真空镀膜机20和基材11均与实施例1中的相同。
溅镀打底层13：钛靶23的功率为10kw，氩气流量为150sccm，基材11的偏压为-100V，镀膜温度为120℃，镀膜时间为5min；该打底层13的厚度为70nm；
溅镀抗菌层15：钛靶23的功率为8kw，铜靶24的功率为5kw，氩气流量为150sccm，基材11的偏压为-100V，镀膜温度为120℃，镀膜时间为20min；该抗菌层15的厚度为950nm。
溅镀防氧化层17：钛靶23的功率为8kw，基材11的偏压为-100V，氩气流量为150sccm，镀膜温度为120℃，镀膜时间为5min；该防氧化层17的厚度为50nm。
抗菌性能测试
将上述制得的抗菌镀膜件10进行抗菌性能测试，抗菌测试参照HG/T3950-2007标准进行，具体测试方法如下：取适量菌液滴于实施例所制得的抗菌镀膜件10和未处理的不锈钢样品上，用灭菌覆盖膜覆盖抗菌镀膜件10和未处理的不锈钢样品，置于灭菌培养皿中，在温度为37±1℃，相对湿度RH>90%的条件下培养24h。然后取出，用20ml洗液反复冲洗样品及覆盖膜，摇匀后取洗液接种于营养琼脂培养基中，在温度为37±1℃的条件下培养24~48h后活菌计数。
将6种霉菌制成孢子悬液，将抗菌镀膜件10浸泡在所述孢子悬液中，在温度为28℃，相对湿度RH>90%的条件下培养28天。
测试结果：实施例1和2所制得的抗菌镀膜件10对大肠杆菌、沙门氏菌、金黄色葡萄球菌的杀菌率均达到99.99%，长霉等级均为0级。
抗氧化性能测试
在温度为150℃，湿度为100%的条件下加速氧化，测试结果：实施例1和2所制得的抗菌镀膜件10加速氧化60h表面均无明显的氧化现象。
本发明所述抗菌镀膜件10的抗菌层15为铜膜和钛膜的交替多层膜，所述抗菌层15中铜膜起抗菌作用，钛膜可起防氧化的作用，同时钛膜可缓释抗菌层15中铜离子的溶出，使抗菌层15具有长效的抗菌效果，相应延长抗菌镀膜件10的使用寿命。

Claims (12)

1.一种抗菌镀膜件，其包括基材，其特征在于：该抗菌镀膜件还包括形成于基材表面的抗菌层及形成于抗菌层表面的防氧化层，该抗菌层包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布。
2.如权利要求1所述的抗菌镀膜件，其特征在于：所述基材的材质为不锈钢。
3.如权利要求1所述的抗菌镀膜件，其特征在于：所述抗菌镀膜件还包括形成于基材与抗菌层之间的打底层。
4.如权利要求3所述的抗菌镀膜件，其特征在于：所述打底层为金属钛层，其以磁控溅射的方式形成，厚度为50～100nm。
5.如权利要求1所述的抗菌镀膜件，其特征在于：与所述打底层结合的为铜膜或钛膜，与所述防氧化层结合的为铜膜或钛膜。
6.如权利要求1所述的抗菌镀膜件，其特征在于：所述抗菌层以磁控溅射的方式形成，其厚度为0.7～1.5μm。
7.如权利要求1所述的抗菌镀膜件，其特征在于：所述防氧化层为金属钛层，其以磁控溅射的方式形成，厚度为20～100nm。
8.一种抗菌镀膜件的制备方法，其包括如下步骤：
提供基材；
在该基材的表面形成抗菌层，该抗菌层包括若干铜膜和若干钛膜，且该若干铜膜和若干钛膜为交替排布；
在该抗菌层的表面形成防氧化层。
9.如权利要求8所述抗菌镀膜件的制备方法，其特征在于：所述抗菌镀膜件的制备方法还包括在形成抗菌层前在基材表面形成打底层。
10.如权利要求9所述抗菌镀膜件的制备方法，其特征在于：形成打底层的步骤采用如下方式实现：采用磁控溅射法，使用钛靶，钛靶的功率为5～10kw，以氩气为工作气体，氩气流量为100～300sccm，对基材施加偏压为-50～-250V，镀膜温度为50～250℃，镀膜时间为5～10min。
11.如权利要求8所述抗菌镀膜件的制备方法，其特征在于：形成所述抗菌层的步骤采用如下方式实现：采用磁控溅射法，使用钛靶和铜靶，钛靶的功率为5～10kw，铜靶的功率为2～8kw，以氩气为工作气体，氩气流量为100～300sccm，对基材施加偏压为-50～-250V，镀膜温度为50～250℃，镀膜时间为10～30min。
12.如权利要求8所述抗菌镀膜件的制备方法，其特征在于：形成所述防氧化层的步骤采用如下方式实现：采用磁控溅射法，使用钛靶，钛靶的功率为5～10kw，以氩气为工作气体，氩气流量为100～300sccm，对基材施加偏压为-50～-250V，镀膜温度为50～250℃，镀膜时间为1～10min。
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