TWI547366B - 具有硬質膜層的不銹鋼製品及其製備方法 - Google Patents

具有硬質膜層的不銹鋼製品及其製備方法 Download PDF

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TWI547366B
TWI547366B TW102103214A TW102103214A TWI547366B TW I547366 B TWI547366 B TW I547366B TW 102103214 A TW102103214 A TW 102103214A TW 102103214 A TW102103214 A TW 102103214A TW I547366 B TWI547366 B TW I547366B
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stainless steel
steel substrate
hard
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張春杰
劉旭
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富智康（香港）有限公司
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    • 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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Description

具有硬質膜層的不鏽鋼製品及其製備方法
本發明涉及一種具有硬質膜層的不銹鋼製品及其製備方法。
現代社會人們對電子產品的質量要求越來越高，不僅要求比較高的外觀質量，同時還要經久耐用，這就要求電子產品表面要有比較高的硬度和耐磨性。
真空鍍膜(PVD)係一種非常環保的鍍膜技術，已被廣泛用來進行材料表面改性，提升材料表面性能。濺射沉積係真空鍍膜方法的一種，其被廣泛用於沉積硬質塗層。係然濺射沉積獲得的塗層的緻密度不夠高，因此限制了塗層硬度的進一步提高。
鑒於此，提供一種具有硬質膜層的不銹鋼製品，該不銹鋼製品具有較高硬度。
另外，還有必要提供一種上述不銹鋼製品的製備方法。
一種具有硬質膜層的不銹鋼製品，其包括不銹鋼基體、依次形成在不銹鋼基體上的打底層、過渡層及硬質層，該打底層為Ti層；該過渡層為TiaCrb層，其中，1≦a≦2、2≦b≦3；該硬質層為TixCryNz層，其中，2≦x≦4、3≦y≦8及10≦z≦16。
一種具有硬質膜層的不銹鋼製品的製備方法，其包括如下步驟： 提供不銹鋼基體；提供一真空鍍膜裝置，該真空鍍膜裝置包括一鍍膜室、設置在該鍍膜室內的鈦靶、鉻靶及射頻電極，該射頻電極用以離化金屬原子及氣體；將該不銹鋼基體置於該真空鍍膜裝置內，開啟所述鈦靶，並向該射頻電極通入電流，在不銹鋼基體上形成一打底層，該打底層為Ti層；同時開啟所述鈦靶和鉻靶，在該打底層上形成一過渡層，該過渡層為TiaCrb層，其中，1≦a≦2、2≦b≦3；以氮氣為反應氣體，同時開啟所述鈦靶和鉻靶，在該過渡層上形成一硬質層，該硬質層為TixCryNz層，其中，2≦x≦4、3≦y≦8，10≦z≦16。
經上述處理後製得的不銹鋼製品的表面顯微維氏硬度為800HV0.025~1000HV0.025。所述不銹鋼製品上形成的膜層組織均勻、緻密性高。
10‧‧‧不銹鋼製品
11‧‧‧不銹鋼基體
111‧‧‧離子注入層
13‧‧‧打底層
15‧‧‧過渡層
17‧‧‧硬質層
200‧‧‧真空鍍膜裝置
20‧‧‧鍍膜室
30‧‧‧真空泵
22‧‧‧鈦靶
23‧‧‧鉻靶
26‧‧‧軌跡
27‧‧‧氣源通道
圖1係本發明較佳實施方式不銹鋼製品的剖視示意圖；圖2係本發明較佳實施方式真空鍍膜裝置的示意圖。
請參閱圖1，本發明一較佳實施例的具有硬質塗層的不銹鋼製品10包括不銹鋼基體11、打底層13、過渡層15及硬質層17。
該不銹鋼基體11表層形成有一離子注入層111。所述打底層13形 成於該離子注入層111上。該離子注入層111中主要含有Fe元素、N元素，Fe與N的原子個數比為1：4~1：7。該離子注入層111的厚度為0.1~0.2μm。
該打底層13為Ti層。該打底層13的厚度為0.3~0.5μm。
該過渡層15為TiaCrb層，其形成於打底層13的表面。TiaCrb中，1≦a≦2、2≦b≦3。該過渡層15的厚度為0.5~0.8μm。
該硬質層17為TixCryNz層，其形成於過渡層15的表面。TixCryNz中，2≦x≦4、3≦y≦8及10≦z≦16。該硬質層17的厚度為1.2~1.5μm。
本發明還提供所述具有硬質層的不銹鋼製品的製備方法，主要包括如下步驟：
(1)提供不銹鋼基體11。
(2)對不銹鋼基體11進行離子注入處理。
請結合參見圖2，提供一真空鍍膜裝置200，其包括一鍍膜室20及連接於鍍膜室20的一真空泵30，真空泵30用以對鍍膜室20抽真空。該鍍膜室20內設有轉架(未圖示)、相對設置的二鈦靶22、相對設置的二鉻靶23及固設在該鍍膜室20頂壁上的射頻電極(未圖示)。轉架帶動不銹鋼基體11沿圓形的軌跡26公轉，且不銹鋼基體11在沿軌跡26公轉時亦自轉。每一鈦靶22及每一鉻靶23的兩端均設有氣源通道27，氣體經該氣源通道27進入所述鍍膜室20中。
該射頻電極用以離化從鈦靶22及鉻靶23濺射出的鈦原子、鉻原子，形成鈦等離子體、鉻等離子體；同時還可離化氬氣、氮氣等氣 體，形成氬氣等離子體、氮氣等離子體。
將不銹鋼基體11固定於真空鍍膜機200的鍍膜室20中的轉架上，將該鍍膜室20抽真空至2×10-1Pa~8×10-1Pa，加熱所述鍍膜室20至200~250℃(即離子注入的溫度為200~250℃)，設置該射頻電極的電流為5-8A，施加於不銹鋼基體11上的偏壓為-1300~-1500V；向該鍍膜室20內通入氮氣及氬氣，氬氣的流量為100~200標準毫升/分鐘(sccm)、氮氣的流量為200~600sccm，離子注入時間為20~35min。如此，在不銹鋼基體11的表層形成一離子注入層111。
在該離子注入過程中，射頻電極放電用以離化氬氣、氮氣，形成氬等離子體、氮等離子體。
該離子注入層111中主要含有Fe元素、N元素，Fe元素來自不銹鋼基體11本身，N元素來自被射頻電極離化形成的氮等離子體。該離子注入層111中，Fe與N的原子個數比為1：4~1：7。該離子注入層111的厚度為0.1~0.2μm。所述離子注入層111可提高所述不銹鋼基體11的硬度。
(3)在不銹鋼基體11上沉積一打底層13。
該打底層13為Ti層。設置該射頻電極的電流為5-8A、所述鍍膜室20的溫度為150~200℃(即濺射溫度為150~200℃)，調節氬氣流量至100~200sccm；開啟所述鈦靶的電源，並設定其功率為3~5kw，於不銹鋼基體11上施加-300~-350V的偏壓，沉積打底層13。沉積該打底層13的時間為8~15min。該打底層13的厚度為0.3~0.5μm。
(4)在打底層13上沉積一過渡層15。
保持所述射頻電極的電流不變，調節氬氣流量至100~150sccm，設置所述鍍膜室至150~180℃(即濺射溫度為150~180℃)；同時開啟所述鈦靶及鉻靶的電源，並設定鈦靶功率為5~7kw，鉻靶功率為8~12kw，於不銹鋼基體11上施加-350~-400V的偏壓，沉積過渡層15。沉積該過渡層15的時間為15~25min。
在形成所述過渡層15的過程中，部分從鈦靶22及鉻靶23濺射出的鈦原子、鉻原子被射頻電極離化成等離子體，如此可提高過渡層15與打底層13的結合力、過渡層15的緻密性。
該過渡層15為TiaCrb層，其中，1≦a≦2、2≦b≦3。該過渡層15的厚度為0.5~0.8μm。
(5)在過渡層15上沉積一硬質層17。
保持所述射頻電極的電流、濺射溫度不變，調節氬氣流量至150~200sccm；設定鈦靶功率為4~6kw、鉻靶功率為10~15kw；向通入氮氣，氮氣的流量為300~500sccm；於不銹鋼基體11上施加-1300~-1500V的偏壓，沉積硬質層17。沉積該硬質層17的時間為25~50min。
在形成所述硬質層17的過程中，部分從鈦靶22及鉻靶23濺射出的鈦原子、鉻原子被射頻電極離化成等離子體，提高了硬質層17中Ti原子及Cr原子與N原子之間的鍵合力、硬質層17內組織的均勻性及緻密性，進而提高硬質層17的硬度。
該硬質層17為TixCryNz層，其中，2≦x≦4、3≦y≦8，10≦z≦16。該硬質層17的厚度為1.2~1.5μm。
(6)對所述形成硬質層17的不銹鋼基體11進行液氮冷卻處理。
向鍍膜室20內通入液氮，以3~5℃/min的降溫速率將鍍膜室20內的溫度降至100℃，並保持鍍膜室20內的壓力為2~5Pa；再以5~6℃/min的降溫速率將鍍膜室20內的溫度由100℃降至70℃，並保持鍍膜室20內的壓力為1~2Pa。
所述液氮冷卻處理，可降低不銹鋼基體11與打底層13之間及各膜層之間的應力，提高膜基之間的結合力、不銹鋼製品10的耐刮擦性能。
經上述處理後製得的不銹鋼製品10的表面顯微維氏硬度為800HV0.025~1000HV0.025。所述不銹鋼製品10上形成的膜層均勻、緻密性高。
實施例1
(1)提供一不銹鋼基體11。
(2)對不銹鋼基體11進行離子注入處理。
所述鍍膜室20內的真空度為2×10-1Pa，離子注入的溫度為220℃，射頻電極的電流6A，施加於不銹鋼基體11上的偏壓為-1400V；氬氣的流量為150sccm、氮氣的流量為400sccm，注入時間為30min。
該離子注入層111的厚度為0.15μm。
(3)在不銹鋼基體11上沉積一打底層13。
保持該射頻電極的電流、氬氣流量不變；設置濺射溫度為170℃、鈦靶的功率為4kw，施加於不銹鋼基體11上的偏壓為-300V，沉 積時間為10min。該打底層13的厚度為0.4μm。
(4)在打底層13上沉積一過渡層15。
保持所述射頻電極的電流、氬氣流量及濺射溫度不變，設置鈦靶的功率為6kw、鉻靶的功率為10kw，施加於不銹鋼基體11上的偏壓為-400V，沉積時間為20min。該過渡層15的厚度為0.6μm。
(5)在過渡層15上沉積一硬質層17.
保持所述射頻電極的電流、濺射溫度不變，設置氬氣流量為180sccm；並設置鈦靶的功率為5kw、鉻靶的功率為12kw；向鍍膜室20通入400sccm流量的氮氣；施加於不銹鋼基體11上的偏壓為-1400V，沉積時間為40min。該硬質層17的厚度為1.4μm。
(6)對所述形成硬質層17的不銹鋼基體11進行液氮冷卻處理。
向鍍膜室20內通入液氮，以3℃/min的降溫速率將鍍膜室20內的溫度降至100℃，並保持鍍膜室20內的壓力為4Pa；再以5℃/min的降溫速率將鍍膜室20內的溫度由100℃降至70℃，並保持鍍膜室20內的壓力為2Pa。
經上述方法形成的不銹鋼製品10的表面顯微維氏硬度為815HV0.025。
實施例2
(1)提供一不銹鋼基體11。
(2)對不銹鋼基體11進行離子注入處理。
所述鍍膜室20內的真空度為5×10-1Pa，離子注入的溫度為250℃， 該射頻電極的電流8A，施加於不銹鋼基體11上的偏壓為-1500V；氬氣的流量為200sccm、氮氣的流量為600sccm，注入時間為30min。
該離子注入層111的厚度為0.15μm。
(3)在不銹鋼基體11上沉積一打底層13。
保持該射頻電極的電流不變，調節氬氣流量至150sccm、濺射溫度為200℃；設置鈦靶的功率為5kw，施加於不銹鋼基體11上的偏壓為-350V，沉積時間為10min。該打底層13的厚度為0.5μm。
(4)在打底層13上沉積一過渡層15。
保持所述射頻電極的電流、氬氣流量及濺射溫度不變，設置鈦靶的功率為7kw、鉻靶的功率為12kw，施加於不銹鋼基體11上的偏壓為-400V，沉積時間為25min。該過渡層15的厚度為0.7μm。
(5)在過渡層15上沉積一硬質層17
保持所述射頻電極的電流、濺射溫度不變，設置氬氣流量至200sccm；設置鈦靶的功率為6kw、鉻靶的功率為15kw；向鍍膜室20通入500sccm流量的氮氣；施加於不銹鋼基體11上的偏壓為-1500V的偏壓，沉積時間為40min。該硬質層17的厚度為1.5μm。
(6)對所述形成硬質層17的不銹鋼基體11進行液氮冷卻處理。
向鍍膜室20內通入液氮，以5℃/min的降溫速率將鍍膜室20內的溫度降至100℃，並保持鍍膜室20內的壓力為4Pa；再以6℃/min的降溫速率將鍍膜室20內的溫度由100℃降至70℃，並保持鍍膜 室20內的壓力為1Pa。
經上述方法形成的不銹鋼製品10的表面顯微維氏硬度為1000HV0.025。
10‧‧‧不銹鋼製品
11‧‧‧不銹鋼基體
111‧‧‧離子注入層
13‧‧‧打底層
15‧‧‧過渡層
17‧‧‧硬質層

Claims (4)

  1. 一種具有硬質膜層的不銹鋼製品的製備方法，其包括如下步驟：提供不銹鋼基體；提供一真空鍍膜裝置，該真空鍍膜裝置包括一鍍膜室、設置在該鍍膜室內的鈦靶、鉻靶及射頻電極，該射頻電極用以離化金屬原子及氣體；將該不銹鋼基體置於該真空鍍膜裝置內，開啟所述鈦靶，並向該射頻電極通入電流，在不銹鋼基體上形成一打底層，該打底層為Ti層；同時開啟所述鈦靶和鉻靶，在該打底層上形成一過渡層，該過渡層為TiaCrb層，其中，1≦a≦2、2≦b≦3；以氮氣為反應氣體，同時開啟所述鈦靶和鉻靶，在該過渡層上形成一硬質層，該硬質層為TixCryNz層，其中，2≦x≦4、3≦y≦8，10≦z≦16。
  2. 如申請專利範圍第1項所述之不銹鋼製品的製備方法，其中所述方法還包括在形成所述打底層之前，向該真空鍍膜裝置內通入氬氣及氮氣，在該不銹鋼基體表層形成一離子注入層的步驟。
  3. 如申請專利範圍第2項所述之不銹鋼製品的製備方法，其中在所述離子注入過程中，射頻電極的電流為5~8A，施加於不銹鋼基體上的偏壓為-1300~-1500V；氬氣的流量為100~200sccm、氮氣的流量為200~600sccm，注入時間為20~35min。
  4. 如申請專利範圍第1項所述之不銹鋼製品的製備方法，其中沉積所述硬質層的過程中，鈦靶功率為4~6kw、鉻靶功率為10~15kw；氮氣的流量為300~500sccm；施加於不銹鋼基體上施加的偏壓為-1300~-1500V，沉積時間為25~50min。
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