TW201239112A - Antibacterial article and method for making the same - Google Patents
Antibacterial article and method for making the same Download PDFInfo
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- TW201239112A TW201239112A TW100110299A TW100110299A TW201239112A TW 201239112 A TW201239112 A TW 201239112A TW 100110299 A TW100110299 A TW 100110299A TW 100110299 A TW100110299 A TW 100110299A TW 201239112 A TW201239112 A TW 201239112A
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Description
201239112 六、發明說明: 【發明所屬之技術領域】 [0001] 本發明涉及一種抗菌鑛膜件及其製備方法。 【先前技術】 [0002] 〇 有害細菌的傳播和感染嚴重咸脅著人類的健康,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、^、 Ag等)塗覆於基材上形成抗g鍍财在目前市場上有著廣 泛的應用。該抗菌鑛膜件的殺菌機理為:抗菌鍵膜件在、 使用過程中,抗菌金屬塗層會__出金屬離子如銅 離子、鋅離子’當微量的具有殺陳的金屢離子與細菌 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内蛋 白質上的疏基、氨基發生反應,使蛋白貧活性破壞,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g塗層通常比較薄,抗菌金屬離子流失較 〇 快’且表面硬飯容易磨損,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。 【發明内容】 _]有鑒於此,有必要提供—種㈣效果較為持久的抗菌鐘 膜件。 _5]另外,還有必要提供__種上述抗祕膜件的製備方法。 [_ -種抗菌鍍_,料減材、形成於純表面的打底 層°玄打底層為錄絡合金層,該抗菌錢膜件還包括形成 100110299 表單編號A0101 第3頁/共15頁 1002017362-0 201239112 於打底層表面的複數鎳鉻氮層和複數銅鈽合金層,該複 數鎳鉻氮層和複數銅鈽合金層交替排布,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 膜件的最外層為鎳絡氮層。 [0007] —種抗菌鍍膜件的製備方法,其包括如下步驟: [0008] 提供基材; [0009] 在該基材的表面形成打底層,該打底層為鎳鉻合金層; [0010] 在該打底層的表面形成鎳鉻氮層; [0011] 在該鎳鉻氮層的表面形成銅鈽合金層; [0012] 重複交替形成鎳鉻氮層和銅鈽合金層以形成最外層為鎳 鉻氮層的抗菌鍍膜件。 [0013] 所述抗菌鍍膜件在基材表面交替濺鍍鎳鉻氮層和銅鈽合 金層,鎳鉻氮層形成為疏鬆多孔的結構,可使銅鈽合金 層的部分嵌入到該鎳鉻氮層中,對銅鈽合金層中銅離子 和鈽離子的快即溶出起到阻礙作用,從而可緩釋銅離子 和飾離子的溶出,使銅鈽合金層具有長效的抗菌效果; 同時錄鉻氮層具有良好的而ί磨性、对腐餘性能,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。 【實施方式】 [0014] 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和複數銅姉合金 100110299 表單編號A0101 第4頁/共15頁 1002017362-0 201239112 (Cu-Ce)層17,該複數鎳鉻氮層15和複數銅鈽合金層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1〇的最外層為鎳鉻氮層15。所述複數 錦絡氮層15和複數銅鈽合金層17的總厚度為2〜3. 2/zm 。本實施例中’所述複數鎳鉻氮層丨5和複數銅鈽合金層 17的層數分別為15〜20層。 [0015] [0016] Ο [0017] ❹ [0018] 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。 該複數鎳絡氮層15可以磁控濺射的方式形成。所述每一 鎳絡氮層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。藏鍵該錄鉻氮層 ! 15時採用較低的沉積溫度和沉稂偏壓’使錄鉻氮層15具 有更好的疏鬆多孔的結構’可使所述銅飾合金層17的部 分嵌入到該銅姉谷金層Η中。 該複數銅鈽合金層17可以磁控濺射的方式形成。所述每 一銅铈合金層17的厚度為40〜8〇nm。銅铈合金層17中釋 放出的銅離子及铈離子均具有穿透細菌的細胞壁並殺死 細菌的能力。在每一銅鈽合金層17與相鄰的每一鎳鉻氮 層15的界面處,有部分銅鈽合金層17嵌入到鎳鉻氮層15 中,從而使銅鈽合金層17固持於鎳鉻氮層15中,可緩釋 銅鈽合金層17中金屬銅和鈽離子的溶出,使銅鈽合金層 100110299 表單編號A0101 第5頁/共15頁 1002017362-0 201239112 17具有長效的抗菌效果。 [0019] 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: [0020] 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。 [0021] 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。 [0022] 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内設有轉架(未圖示)、二鎳鉻合金靶23和二銅 鈽合金靶24。轉架帶動基材11沿圓形的執跡25公轉,且 基材11在沿轨跡25公轉時亦自轉。 [0023] 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内,將該鍍膜室21抽真空至3x 10 5torr,然後向鍍膜室内通入流量為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3〜1 0miη。 [0024] 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 100110299 表單編號Α0101 第6頁/共15頁 1002017362-0 201239112 層13在所述真空鍍膜機2〇中進行。使用鎳鉻合金靶23, 所述錄絡合金靶23中鎳的質量百分含量為2〇〜40%,其採 用直流磁控電源。濺鍍時,開啟鎳鉻合金靶23,設置鎳 鉻合金乾23的功率為7〜llkw ’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 歷,鑛膜溫度為70〜90°C,鍍膜時間為5〜lOmin。該打 底層13的厚度為150〜250nm。 [0025] ❹ 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,開啟錄鉻合金把含3 ’設置鎳鉻 合金靶23的功率為7〜llkw,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4〇〇 〜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70〜9〇°C,鍍膜時間為5〜 G [0026] 7min。該鎳鉻氮層15的厚異為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,可使錄路 氮層15達到較好的疏鬆多孔的結構。 繼續採用磁控賤射法在所述鎳鉻氮層15的表面激鑛銅鈽 合金層17。使用銅飾合金把24,所述鋼鈽合金乾24中銅 的質量百分含量為88〜95%,其採用直流磁控電源。濺鍍 時’開啟銅飾合金乾24,設置銅飾合金乾24的功率為8〜 10kw ’通入工作氣體氬氣,氬氣流量為4〇〇〜5〇〇sccm, 對基材11施加直流偏壓,直流偏壓大小為-50〜_1〇〇v, 鑛膜/皿度為70〜9〇C,鑛膜時間為5〜7min。該銅鈽合 金層17的厚度為4〇〜8〇nm。 100110299 表單編號A0101 第7頁/共15頁 1002017362-0 201239112 [0027] 參照上述步驟,重複交替濺鍍鎳鉻氮層15和銅鈽合金層 17,且使抗菌鑛膜件10的最外層為鎳鉻氮層15。交替滅 鍍的次數總共為15〜20次。所述複數鎳鉻氮層15和複數 銅飾合金層17的總厚度為2〜3. 2/zm。 [0028] 下面藉由實施例來對本發明進行具體說明。 [0029] 實施例1 [0030] 本實施例所使用的真空鍍膜機20為磁控濺射鍍膜機。 [0031] 本實施例所使用的基材11的材質為不銹鋼。 [0032] 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 ; [0033] 濺鍍打底層13 :鎳鉻合金靶23中鎳的質量百分含量為35% ,錄鉻合金把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°C,鍍膜時間為 6min ;該打底層13的厚度為185nm ; [0034] 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°C,鍍膜時間為7min ;該鎳鉻氮層的厚 度為75nm。 [0035] 濺鍍銅鈽合金層1 7 :銅鈽合金靶24中銅的質量百分含量 為88%,銅鈽合金靶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°C,鍍膜時間 為7min ;該銅錦合金層17的厚度為70nm。 [0036] 重複交替濺鍍鎳鉻氮層15和銅鈽合金層17的步驟,濺鍍 100110299 表單編號A0101 第8頁/共15頁 1002017362-0 201239112 鎳鉻氮層15的次數為17次,濺鑛銅鈽合金層17的次數為 16次。 [0037] 實施例2 [0038] 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。 [0039] 電聚清洗:氬氣流量為500sccm,基材11的偏壓為-200V ,電漿清洗時間為5 in i η ; [0040] 濺鍍打底層13 :鎳鉻合金靶23中鎳的質量百分含量為40% ,錄鉻合金乾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°C,鍍膜時間為 5min ;該打底層13的厚度為185nm ; [0041] 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lOOsccm,基材11的偏壓為-80V,鍍膜溫度為80°C,鍍膜時間為5min ;該鎳鉻氮層 的厚度為60nm 〇 [0042] 濺鍍銅鈽合金層17 :銅鈽合金靶24中銅的質量百分含量 為95%,銅鈽合金靶24的功率為8kw,基材11的偏壓為-80V,氬氣流量為400sccm,鑛膜溫度為80°C,鑛膜時間 為5min ;該銅飾合金層17的厚度為65nm。 [0043] 重複交替滅鍍錄鉻氮層15和銅鈽合金層17的步驟,滅鍍 鎳鉻氮層15的次數為17次,激鍵銅鈽合金層17的次數為 1 6次。 [0044] 抗菌性能測試 1002017362-0 100110299 表單編號A0101 第9頁/共15頁 201239112 [0045] 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/T3950-20 07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1 〇和未處理 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,置於滅菌培養孤中,在溫度為37±1 °C,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°C下培養24〜48h後 進行活菌計數。 [0046] 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°C,相對濕度RH>90%的條件下培 養28天。 [0047] 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98. 5%, 長霉等級均為1級。 [0048] 抗菌持久性測試:經過在溫度為37±1PC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大於97. 3%, 長霉等級均為1級。 [0049] 所述抗菌鍍膜件10在基材11表面交替濺鍍鎳鉻氮層15和 銅鈽合金層17,鎳鉻氮層15形成為疏鬆多孔的結構,可 使銅鈽合金層17的部分嵌入到該鎳鉻氮層15中,對銅鈽 合金層1 7中銅離子和鈽離子的快即溶出起到阻礙作用, 100110299 表單編號A0101 第10頁/共15頁 1002017362-0 201239112 從而可緩釋銅離子和鈽離子的溶出,使銅鈽合金層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#性能,因而在整個膜層的最外層鑛上錄鉻氮層 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。 【圖式簡單說明】 [0050] 圖1為本發明一較佳實施例的抗菌鍍膜件的剖視圖; [0051] 圖2為本發明一較佳實施例真空鍍膜機的俯視示意圖。
[0052] 【主要元件符號說明】 抗菌鍍膜件:10 [0053] 基材:11 [0054] 打底層:13 [0055] 鎳鉻氮層:15 [0056] 銅铈合金層:17 [0057] 真空鍍膜機:20 [0058] 鍍膜室:21 [0059] 鎳鉻合金靶:23 [0060] 銅鈽合金靶:24 [0061] 軌跡:25 [0062] 真空泵:30 100110299 表單編號A0101 第11頁/共15頁 1002017362-0
Claims (1)
- 201239112 七、申請專利範圍: 1 . 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鈽合金層 ,該複數鎳鉻氮層和複數銅鈽合金層交替排布,且與所述 打底層直接相結合的係鎳鉻氮層,該抗菌鑛膜件的最外層 為鎳鉻氮層。 2 .如申請專利範圍第1項所述之抗菌鍍膜件,其中所述基材 的材質為不錄鋼。 3 .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。 4 .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 〇 5 .如申請專利範圍第1項所述之抗菌鍍膜件,其中所述複數 銅鈽合金層以磁控濺射的方式形成,每一銅鈽合金層的厚 度為40〜80nm。 6 .如申請專利範圍第1項所述之抗菌鍍膜件,其中所述複數 鎳鉻氮層和複數銅鈽合金層的總厚度為2〜3. 2 # m。 7 . —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鈽合金層; 100110299 表單編號A0101 第12頁/共15頁 1002017362-0 201239112 重複交替形成鎳鉻氮層和銅鈽合金層以形成最外層為鎳鉻 氮層的抗菌鑛膜件。 8 .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〜llkw,以氬氣 為工作氣體,氣氣流量為350〜500sccm,對基材施加偏 壓為-100〜-150V,鍍膜溫度為70〜90°C,鍍膜時間為5 〜1 0miη 〇 Ο 9 .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〜llkw,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°C,鍍膜時間為5〜 7min ° C) 10 .如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其 中形成所述銅鈽合金層的步驟採用如下方式實現:採用磁 控濺射法,使用銅鈽合金靶,所述銅鈽合金靶中銅的質量 百分含量為88〜95%,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°C,鍍膜時間為5〜7min。 11 .如申請專利範圍第7項所述之抗菌鍍膜件的製備方法,其 中所述交替形成錄鉻氮層和銅鋪合金層的次數總共為1 5〜 20次。 100110299 表單編號A0101 第13頁/共15頁 1002017362-0
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