TWI417409B - 鍍膜件及其製造方法 - Google Patents
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Description
本發明涉及一種鍍膜件及其製造方法,尤其涉及一種具有Si-B-C-N陶瓷層的鍍膜件及其製造方法。
Si-B-C-N複合陶瓷材料由於其具有高硬度、低密度及優異的高溫穩定性、抗氧化性、機械性能等性能,可應用於高溫、高壓、高頻等極端條件下,引起了人們對其極大地關注。
習知技術,用於製造Si-B-C-N複合陶瓷的主要方法如下:熱壓燒結法、反應燒結法、原位合成法及前驅體法等。前驅體法由於其具有燒結溫度低、原子尺寸可控性佳的優點而被人們廣泛應用,但同時前驅體法亦存在一定的缺陷如:選取氯矽烷為原料時,易產生難以去除的副產品氯化銨;選取硼烷為原料時難以摻入硼元素;上述兩種情況都將影響Si-B-C-N複合陶瓷的性能。此外,選用某些含硼有機物為原料製備出的Si-B-C-N複合陶瓷雖然具有較佳的性能,但存在製造工藝複雜、實驗條件苛刻等缺點。
鑒於此,本發明提供一種可克服上述問題的具有Si-B-C-N陶瓷層的鍍膜件。
另外,本發明還提供一種上述鍍膜件的製造方法。
一種鍍膜件,包括基體及藉由磁控濺射鍍膜法形成於基體上的Si-B-C-N陶瓷層,該Si-B-C-N陶瓷層為非晶態層,該Si-B-C-N陶瓷層中Si的質量百分含量為30~60%,B的質量百分含量為10~20%,C的質量百分含量為10~20%,N的質量百分含量為20~30%。
一種鍍膜件的製造方法,其包括如下步驟:提供基體;藉由磁控濺射鍍膜法,以Si-B-N靶為靶材,以乙炔為反應氣體在該基體的表面形成Si-B-C-N陶瓷層,該Si-B-C-N陶瓷層為非晶態層,該Si-B-C-N陶瓷層中Si的質量百分含量為30~60%,B的質量百分含量為10~20%,C的質量百分含量為10~20%,N的質量百分含量為20~30%。
本發明所述Si-B-C-N陶瓷層中B元素的引入係藉由磁控濺射Si-B-N靶實現的,幾乎沒有副產物的產生或雜質的帶入,且製造方法簡單,如此使Si-B-C-N陶瓷材料在高溫抗氧化領域具有廣泛的應用前景。
經上述方式形成的Si-B-C-N陶瓷層為緻密的非晶態層,且該Si-B-C-N陶瓷層中含有較多的Si-C,Si-N,C-N等共價鍵,使所述Si-B-C-N陶瓷層具有良好的抗氧化性,從而提高了所述鍍膜件的抗氧化性。進一步地,由於B元素的加入可提高該Si-B-C-N陶瓷層的析晶溫度,使該Si-B-C-N陶瓷層在較高的溫度下仍可保持非晶態結構,如此,使所述鍍膜件具有良好的高溫抗氧化性。
10‧‧‧鍍膜件
11‧‧‧基體
13‧‧‧Si-B-C-N陶瓷層
20‧‧‧真空鍍膜機
21‧‧‧鍍膜室
23‧‧‧Si-B-N靶
25‧‧‧軌跡
30‧‧‧真空泵
圖1係本發明一較佳實施例鍍膜件的剖視圖;
圖2係本發明一較佳實施例真空鍍膜機的示意圖。
請參閱圖1,本發明一較佳實施例的鍍膜件10包括基體11及形成於基體11表面的矽-硼-碳-氮(Si-B-C-N)陶瓷層13。該鍍膜件10可為渦輪葉片、噴嘴等航天航空機械零部件及交通零部件。
基體11的材質為金屬,優選為不銹鋼、鋁或鋁合金,但不限於上述材料。
所述Si-B-C-N陶瓷層13為緻密的非晶態層。其中,Si的質量百分含量為30~60%,B的質量百分含量為10~20%,C的質量百分含量為10~20%,N的質量百分含量為20~30%。該Si-B-C-N陶瓷層13的厚度為100~1000nm。該Si-B-C-N陶瓷層13藉由磁控濺射鍍膜法形成。
本發明鍍膜件10的製造方法包括以下步驟:提供基體11,該基體11的材質為金屬,該金屬可為不銹鋼、鋁或鋁合金等,但不限於上述材料。
將基體11放入無水乙醇中進行超聲波清洗,以去除基體11表面的污漬,清洗時間可為30~50min。
對經上述處理後的基體11的表面進行電漿清洗,以進一步去除基體11表面的油污,以及改善基體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)和相對設置的二Si-B-N靶23。轉架帶動基體11沿圓形的軌跡25公轉,且基體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可為:將基體11固定於真空鍍膜機20的鍍膜室21中的轉架上,將該鍍膜室21抽真空至3.0×10-5Torr,然後向鍍膜室21內通入流量約為500sccm(標準狀態毫升/分鐘)的氬氣(純度為99.999%),並施加-200~-500V的偏壓於基體11,對基體11的表面進行電漿清洗,清洗時間為3~10min。
採用磁控濺射鍍膜法,在經電漿清洗後的基體11上濺鍍Si-B-C-N陶瓷層13。濺鍍該Si-B-C-N陶瓷層13在所述真空鍍膜機20中進行。開啟Si-B-N靶23,並設定Si-B-N靶23的功率為3~5kw;以乙炔為反應氣體,調節乙炔的流量為10~100sccm,以氬氣為工作氣體,調節氬氣的流量為300~500sccm。濺鍍時,對基體11施加-50~-180V的偏壓,並加熱所述鍍膜室21至溫度為50~100℃(即鍍膜溫度為50~100℃),鍍膜時間可為20~60min。該Si-B-C-N陶瓷層13的厚度可為100~1000nm。
可以理解的,本發明所述鍍膜件10還可在基體11與Si-B-C-N陶瓷層13之間設置一打底層,以增加膜基結合力。
其中,所述Si-B-N靶23中Si的質量百分含量為12~45%,B的質量百分含量為10~35%,N的質量百分含量為40~55%。所述Si-B-N靶23藉由粉末冶金的方法製得,其具體步驟及工藝參數如下:
(1)將氮化硼(BN)或硼(B)與氮化矽(Si3N4)的混合粉體原料放入球磨機中混合均勻;其中,BN或B與Si3N4的摩爾比為1:1~50,優選為1:1~20,更佳優選為1:3。
(2)採用冷等靜壓法,將上述混合粉體進行預壓成型形成一坯
體,成型壓力100~300MPa,保壓時間1~10min。
(3)將上述坯體置入放電等離子體(SPS)燒結爐中進行燒結。在該燒結過程中,先以90~100℃/min速率進行升溫,當溫度升高到800~900℃時進行預壓,預壓壓力為20~40MPa,預壓時間為1~5min;預壓後,將溫度上升到900~1500℃,於50~70MPa壓力下保壓3~10min;降溫後取出得到Si-B-N靶23。
本發明所述Si-B-C-N陶瓷層13中B元素的引入係藉由磁控濺射Si-B-N靶實現的,幾乎沒有副產物的產生或雜質的帶入,且製造方法簡單,如此使Si-B-C-N陶瓷材料在高溫抗氧化領域具有廣泛的應用前景。
經上述方式形成的Si-B-C-N陶瓷層13為緻密的非晶態層,且該Si-B-C-N陶瓷層13中含有較多的Si-C,Si-N,C-N等共價鍵,使所述Si-B-C-N陶瓷層13具有良好的抗氧化性,從而提高了所述鍍膜件10的抗氧化性。進一步地,由於B元素的加入可提高該Si-B-C-N陶瓷層13的析晶溫度,使該Si-B-C-N陶瓷層13在較高的溫度下仍可保持非晶態結構,如此,使所述鍍膜件10具有良好的高溫抗氧化性。
10‧‧‧鍍膜件
11‧‧‧基體
13‧‧‧Si-B-C-N陶瓷層
Claims (4)
- 一種鍍膜件的製造方法,其包括如下步驟:提供基體;採用磁控濺射鍍膜法,以Si-B-N靶為靶材,以乙炔為反應氣體在該基體的表面形成Si-B-C-N陶瓷層,該Si-B-C-N陶瓷層為非晶態層,該Si-B-C-N陶瓷層中Si的質量百分含量為30~60%,B的質量百分含量為10~20%,C的質量百分含量為10~20%,N的質量百分含量為20~30%。
- 如申請專利範圍第1項所述之鍍膜件的製造方法,其中所述Si-B-N靶以如下方式製備:將氮化硼或硼與氮化矽的混合粉體原料放入球磨機中混合均勻;其中,氮化硼或硼與氮化矽的摩爾比為1:1~50;採用冷等靜壓,將上述混合粉體進行預壓成型形成一坯體,成型壓力100~300MPa,保壓時間1~10min;將上述坯體置入放電等離子體燒結爐中進行燒結,在該燒結過程中,先以90~100℃/min速率進行升溫,當溫度升高到800~900℃時進行預壓,預壓壓力為20~40MPa,預壓時間為1~5min;預壓後,將溫度上升到900~1500℃,於50~70MPa壓力下保壓3~10min;降溫後取出得到Si-B-N靶。
- 如申請專利範圍第2項所述之鍍膜件的製造方法,其中所述Si-B-N靶中Si的質量百分含量為12~45%,B的質量百分含量為10~35%,N的質量百分含量為40~55%。
- 如申請專利範圍第1項所述之鍍膜件的製造方法,其中形成 所述Si-B-C-N陶瓷層的工藝參數為:Si-B-N靶的功率為3~5kw,乙炔的流量為10~100sccm,以氬氣為工作氣體,氬氣的流量為300~500sccm,施加於基體的偏壓為-50~-180V,鍍膜溫度為5~100℃,鍍膜時間為20~60min。
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US20100304102A1 (en) * | 2005-11-04 | 2010-12-02 | Metaplas Ionon Oberflaechenveredelungstechnik Gmbh | Layer arrangement for the formation of a coating on a surface of a substrate, coating method, and substrate with a layer arrangement |
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