TWI428458B - 抗菌鍍膜件及其製備方法 - Google Patents
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Description
本發明涉及一種抗菌鍍膜件及其製備方法。
有害細菌的傳播和感染嚴重威脅著人類的健康,尤其近年來SARS病毒、禽流感等的傳播和感染,使抗菌材料在日常生活中的應用迅速發展起來。將抗菌金屬(Cu、Zn、Ag等)塗覆於基材上形成抗菌鍍膜件在目前市場上有著廣泛的應用。該抗菌鍍膜件的殺菌機理為抗菌鍍膜件在使用過程中,抗菌金屬塗層會緩慢釋放出金屬離子如銅離子、鋅離子,當微量的具有殺菌性的金屬離子與細菌等微生物接觸時,該金屬離子依靠庫倫力與帶有負電荷的微生物牢固吸附,金屬離子穿透細胞壁與細菌體內蛋白質上的巰基、氨基發生反應,使蛋白質活性破壞,使細胞喪失分裂增殖能力而死亡,從而達到殺菌的目的。
然該類金屬抗菌塗層通常比較薄,抗菌金屬離子流失較快,且表面硬度較低容易磨損,從而降低了金屬抗菌塗層的抗菌持久性,甚至使抗菌塗層失去抗菌效果。
有鑒於此,有必要提供一種抗菌效果較為持久的抗菌鍍膜件。
另外,還有必要提供一種上述抗菌鍍膜件的製備方法。
一種抗菌鍍膜件,其包括基材、形成於基材表面的打底層,該打底層為鎳鉻合金層,該抗菌鍍膜件還包括形成於打底層表面的複數鎳鉻氮層和複數銅鋅合金層,該複數鎳鉻氮層和複數銅鋅合金層交替排布,該抗菌鍍膜件中與所述打底層直接相結合的係鎳鉻氮層,且該抗菌鍍膜件的最外層為鎳鉻氮層。
一種抗菌鍍膜件的製備方法,其包括如下步驟:提供基材;在該基材的表面形成打底層,該打底層為鎳鉻合金層;在該打底層的表面形成鎳鉻氮層;在該鎳鉻氮層的表面形成銅鋅合金層;重複交替形成鎳鉻氮層和銅鋅合金層以形成最外層為鎳鉻氮層的抗菌鍍膜件。
所述抗菌鍍膜件在基材表面交替濺鍍鎳鉻氮層和銅鋅合金層,鎳鉻氮層形成為疏鬆多孔的結構,可使銅鋅合金層的部分嵌入到該鎳鉻氮層中,對銅鋅合金層中銅和鋅離子的快即溶出起到阻礙作用,從而可緩釋銅和鋅離子的溶出,使銅鋅合金層具有長效的抗菌效果;同時鎳鉻氮層具有良好的耐磨性、耐腐蝕性能,因而在整個膜層的最外層鍍上鎳鉻氮層有助於提升抗菌鍍膜件的耐磨性,可延長抗菌鍍膜件的使用壽命。
10‧‧‧抗菌鍍膜件
11‧‧‧基材
13‧‧‧打底層
15‧‧‧鎳鉻氮層
17‧‧‧銅鋅合金層
20‧‧‧真空鍍膜機
21‧‧‧鍍膜室
23‧‧‧鎳鉻合金靶
24‧‧‧銅鋅合金靶
25‧‧‧軌跡
30‧‧‧真空泵
圖1為本發明一較佳實施例的抗菌鍍膜件的剖視圖;圖2為本發明一較佳實施例真空鍍膜機的俯視示意圖。
請參閱圖1,本發明一較佳實施方式的抗菌鍍膜件10包括基材11、形成於基材11表面的打底層13,形成於打底層13表面的複數鎳鉻氮(NiCrN)層15和複數銅鋅合金(Cu-Zn)層17,該複數鎳鉻氮層15和複數銅鋅合金層17交替排布,其中與所述打底層13直接相結合的係鎳鉻氮層15,抗菌鍍膜件10的最外層為鎳鉻氮層15。所述複數鎳鉻氮層15和複數銅鋅合金層17的總厚度為2~3.2μm。本實施例中,所述複數鎳鉻氮層15和複數銅鋅合金層17的層數分別為15~20層。
該基材11的材質優選為不銹鋼,但不限於不銹鋼。
該打底層13可以磁控濺射的方式形成。該打底層為一鎳鉻合金層。該打底層13的厚度為150~250nm。
該複數鎳鉻氮層15可以磁控濺射的方式形成。所述每一鎳鉻氮層15的厚度為40~80nm。所述鎳鉻氮層15中鎳的原子百分含量為30~45%,鉻的原子百分含量為40~55%,氮的原子百分含量為5~15%;該種質量百分比例的鎳鉻氮層15具有較高的硬度和良好的耐磨性。濺鍍該鎳鉻氮層15時採用較低的沉積溫度和沉積偏壓,使鎳鉻氮層15具有更好的疏鬆多孔的結構,可使所述銅鋅合金層17的部分嵌入到該鎳鉻氮層15中。
該複數銅鋅合金層17可以磁控濺射的方式形成。所述每一銅鋅合
金層17的厚度為40~80nm。在每一銅鋅合金層17與相鄰的每一鎳鉻氮層15的界面處,有部分銅鋅合金層17嵌入到鎳鉻氮層15中,從而使銅鋅合金層17固持於鎳鉻氮層15中,可緩釋銅鋅合金層17中銅和鋅離子的溶出,使銅鋅合金層17具有長效的抗菌效果。
本發明一較佳實施方式的抗菌鍍膜件10的製備方法,其包括如下步驟:提供基材11,該基材11的材質優選為不銹鋼,但不限於不銹鋼。
對該基材11進行表面預處理。該表面預處理可包括常規的對基材11進行拋光、無水乙醇超聲波清洗及烘乾等步驟。
對經上述處理後的基材11的表面進行氬氣電漿清洗,以進一步去除基材11表面殘留的雜質,以及改善基材11表面與後續鍍層的結合力。結合參閱圖2,提供一真空鍍膜機20,該真空鍍膜機20包括一鍍膜室21及連接於鍍膜室21的一真空泵30,真空泵30用以對鍍膜室21抽真空。該鍍膜室21內設有轉架(未圖示)、一鎳鉻合金靶23和一銅鋅合金靶24。轉架帶動基材11沿圓形的軌跡25公轉,且基材11在沿軌跡25公轉時亦自轉。
該電漿清洗的具體操作及工藝參數為:將基材11放入一真空鍍膜機20的鍍膜室21內,將該鍍膜室21抽真空至3×10-5torr,然後向鍍膜室內通入流量為500sccm(標準狀態毫升/分鐘)的氬氣(純度為99.999%),並施加-200~-350V的偏壓於基材11,對基材11表面進行氬氣電漿清洗,清洗時間為3~10min。
採用磁控濺射法在經氬氣電漿清洗後的基材11的表面濺鍍打底層
13,該打底層13為一鎳鉻合金層。濺鍍該打底層13在所述真空鍍膜機20中進行。使用鎳鉻合金靶23,所述鎳鉻合金靶23中鎳的質量百分含量為20~40%,其採用直流磁控電源。濺鍍時,開啟鎳鉻合金靶23,設置鎳鉻合金靶23的功率為7~11kw,通入工作氣體氬氣,氬氣流量為350~500sccm,對基材11施加-100~-150V的偏壓,鍍膜溫度為70~90℃,鍍膜時間為5~10min。該打底層13的厚度為150~250nm。
繼續採用磁控濺射法在所述打底層13的表面濺鍍鎳鉻氮層15。繼續使用鎳鉻合金靶23,所述鎳鉻合金靶23採用直流磁控電源。濺鍍時,開啟鎳鉻合金靶23,設置鎳鉻合金靶23的功率為7~11kw,通入反應氣體氮氣,氮氣流量為45~120sccm,通入工作氣體氬氣,氬氣流量為400~500sccm,對基材11施加直流偏壓,直流偏壓大小為-50~-100V,鍍膜溫度為70~90℃,鍍膜時間為5~7min。該鎳鉻氮層15的厚度為40~80nm。濺鍍該鎳鉻氮層15採用較低的沉積溫度和較低的沉積偏壓,可使鎳鉻氮層15達到較好的疏鬆多孔的結構。
繼續採用磁控濺射法在所述鎳鉻氮層15的表面濺鍍銅鋅合金層17。使用銅鋅合金靶24,所述銅鋅合金靶24中銅的質量百分含量為65%~76%,其採用直流磁控電源。濺鍍時,開啟銅鋅合金靶24,設置銅鋅合金靶24的功率為8~10kw,通入工作氣體氬氣,氬氣流量為400~500sccm,對基材11施加直流偏壓,直流偏壓大小為-50~-100V,鍍膜溫度為70~90℃,鍍膜時間為5~7min。該銅鋅合金層17的厚度為40~80nm。
參照上述步驟,重複交替濺鍍鎳鉻氮層15和銅鋅合金層17,且使抗菌鍍膜件10的最外層為鎳鉻氮層15。交替濺鍍的次數總共為15~20次。所述複數鎳鉻氮層15和複數銅鋅合金層17的總厚度為2~3.2μm。
下面藉由實施例來對本發明進行具體說明。
本實施例所使用的真空鍍膜機20為磁控濺射鍍膜機。
本實施例所使用的基材11的材質為不銹鋼。
電漿清洗:氬氣流量為500sccm,基材11的偏壓為-200V,電漿清洗時間為5min;濺鍍打底層13:鎳鉻合金靶23中鎳的質量百分含量為35%,鎳鉻合金靶23的功率為7kw,氬氣流量為420sccm,基材11的偏壓為-100V,鍍膜溫度為80℃,鍍膜時間為6min;該打底層13的厚度為185nm;濺鍍鎳鉻氮層15:鎳鉻合金靶23的功率為8kw,氬氣流量為400sccm,氮氣流量為60sccm,基材11的偏壓為-80V,鍍膜溫度為80℃,鍍膜時間為7min;該鎳鉻氮層的厚度為75nm。
濺鍍銅鋅合金層17:銅鋅合金靶24中銅的質量百分含量為66%,銅鋅合金靶24的功率為8kw,基材11的偏壓為-80V,氬氣流量為400sccm,鍍膜溫度為80℃,鍍膜時間為7min;該銅鋅合金層17的厚度為70nm。
重複交替濺鍍鎳鉻氮層15和銅鋅合金層17的步驟,濺鍍鎳鉻氮層15的次數為17次,濺鍍銅鋅合金層17的次數為16次。
本實施例所使用的真空鍍膜機20和基材11均與實施例1中的相同。
電漿清洗:氬氣流量為500sccm,基材11的偏壓為-200V,電漿清洗時間為5min;濺鍍打底層13:鎳鉻合金靶23中鎳的質量百分含量為40%,鎳鉻合金靶23的功率為7kw,氬氣流量為420sccm,基材11的偏壓為-100V,鍍膜溫度為80℃,鍍膜時間為5min;該打底層13的厚度為185nm;濺鍍鎳鉻氮層15:鎳鉻合金靶23的功率為7kw,氬氣流量為400sccm,氮氣流量為100sccm,基材11的偏壓為-80V,鍍膜溫度為80℃,鍍膜時間為5min;該鎳鉻氮層的厚度為60nm。
濺鍍銅鋅合金層17:銅鋅合金靶24中銅的質量百分含量為74%,銅鋅合金靶24的功率為8kw,基材11的偏壓為-80V,氬氣流量為400sccm,鍍膜溫度為80℃,鍍膜時間為5min;該銅鋅合金層17的厚度為65nm。
重複交替濺鍍鎳鉻氮層15和銅鋅合金層17的步驟,濺鍍鎳鉻氮層15的次數為17次,濺鍍銅鋅合金層17的次數為16次。
將上述製得的抗菌鍍膜件10進行抗菌性能測試,抗菌測試參照HG/T3950-2007標準進行,具體測試方法如下:取適量菌液滴於實施例所製得的抗菌鍍膜件10和未處理的不銹鋼樣品上,用滅菌覆蓋膜覆蓋抗菌鍍膜件10和未處理的不銹鋼樣品,置於滅菌培養皿中,在溫度為37±1℃,相對濕度為RH>90%的條件下培養24h。然後取出,用20ml洗液反復沖洗樣品及覆蓋膜,搖勻後取洗液接種於營養瓊脂培養基中,在溫度為37±1℃下培養24~48h後進行活菌計數。
將6種霉菌製成孢子懸液,將抗菌鍍膜件10浸泡在所述孢子懸液中,在溫度為28℃,相對濕度RH>90%的條件下培養28天。
測試結果:實施例1和2所製得的抗菌鍍膜件10對大腸桿菌、沙門氏菌、金黃色葡萄球菌的殺菌率均達到99.5%,長黴等級均為1級。
抗菌持久性測試:經過在溫度為37±1℃的恒溫水溶液中浸泡3個月後的抗菌抗菌鍍膜件10,再次進行抗菌性能測試,實施例1和2所製得的抗菌抗菌鍍膜件10對大腸桿菌、沙門氏菌、金黃色葡萄球菌的殺菌率依然達到99.3%,長黴等級均為1級。
所述抗菌鍍膜件10在基材11表面交替濺鍍鎳鉻氮層15和銅鋅合金層17,鎳鉻氮層15形成為疏鬆多孔的結構,可使銅鋅合金層17的部分嵌入到該鎳鉻氮層15中,對銅鋅合金層17中銅和鋅離子的快即溶出起到阻礙作用,從而可緩釋銅和鋅離子的溶出,使銅鋅合金層17具有長效的抗菌效果。同時鎳鉻氮層15具有良好的耐磨性
、耐腐蝕性能,因而在整個膜層的最外層鍍上鎳鉻氮層15有助於提升抗菌鍍膜件10的耐磨性,可延長抗菌鍍膜件10的使用壽命。
10‧‧‧抗菌鍍膜件
11‧‧‧基材
13‧‧‧打底層
15‧‧‧鎳鉻氮層
17‧‧‧銅鋅合金層
Claims (11)
- 一種抗菌鍍膜件,其包括基材、形成於基材表面的打底層,該打底層為鎳鉻合金層,其改良在於:該抗菌鍍膜件還包括形成於打底層表面的複數鎳鉻氮層和複數銅鋅合金層,該複數鎳鉻氮層和複數銅鋅合金層交替排布,且與所述打底層直接相結合的係鎳鉻氮層,該抗菌鍍膜件的最外層為鎳鉻氮層,每一鎳鉻氮層具有疏鬆多孔的結構,使與其相鄰的銅鋅合金層的部分嵌入到該鎳鉻氮層中。
- 如申請專利範圍第1項所述之抗菌鍍膜件,其中所述基材的材質為不銹鋼。
- 如申請專利範圍第1項所述之抗菌鍍膜件,其中所述打底層以磁控濺射的方式形成,該打底層的厚度為150~250nm。
- 如申請專利範圍第1項所述之抗菌鍍膜件,其中所述複數鎳鉻氮層以磁控濺射的方式形成,每一鎳鉻氮層的厚度為40~80nm。
- 如申請專利範圍第1項所述之抗菌鍍膜件,其中所述複數銅鋅合金層以磁控濺射的方式形成,每一銅鋅合金層的厚度為40~80nm。
- 如申請專利範圍第1項所述之抗菌鍍膜件,其中所述複數鎳鉻氮層和複數銅鋅合金層的總厚度為2~3.2μm。
- 一種抗菌鍍膜件的製備方法,其包括如下步驟:提供基材;在該基材的表面形成打底層,該打底層為鎳鉻合金層; 在該打底層的表面形成鎳鉻氮層,該鎳鉻氮層具有疏鬆多孔的結構;在該鎳鉻氮層的表面形成銅鋅合金層,該銅鋅合金層的部分嵌入到該鎳鉻氮層中;重複交替形成鎳鉻氮層和銅鋅合金層以形成最外層為鎳鉻氮層的抗菌鍍膜件。
- 如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其中形成所述打底層的步驟採用如下方式實現:採用磁控濺射法,使用鎳鉻合金靶,所述鎳鉻合金靶中鎳的質量百分含量為20~40%,鎳鉻合金靶的功率為7~11kw,以氬氣為工作氣體,氬氣流量為350~500sccm,對基材施加偏壓為-100~-150V,鍍膜溫度為70~90℃,鍍膜時間為5~10min。
- 如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其中形成所述鎳鉻氮層的步驟採用如下方式實現:採用磁控濺射法,使用鎳鉻合金靶,所述鎳鉻合金靶中鎳的質量百分含量為20~40%,鎳鉻合金靶的功率為7~11kw,以氮氣為反應氣體,氮氣流量為45~120sccm,以氬氣為工作氣體,氬氣流量為400~500sccm,對基材施加偏壓為-50~-100V,鍍膜溫度為70~90℃,鍍膜時間為5~7min。
- 如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其中形成所述銅鋅合金層的步驟採用如下方式實現:採用磁控濺射法,使用銅鋅合金靶,所述銅鋅合金靶中銅的質量百分含量為65%~76%,以氬氣為工作氣體,氬氣流量為400~500sccm,對基材施加偏壓為-50~-100V,鍍膜溫度為70~90℃,鍍膜時間為5~7min。
- 如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其中所述交替形成鎳鉻氮層和銅鋅合金層的次數總共為15~20次。
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