CN106256928B - γ-TiAl合金表面(Al2O3+Y2O3)/AlYMoSi多层结构涂层及其制备方法 - Google Patents
γ-TiAl合金表面(Al2O3+Y2O3)/AlYMoSi多层结构涂层及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种γ‑TiAl合金表面(Al2O3+Y2O3)/AlYMoSi多层结构涂层及其制备方法,该涂层包括表层(Al2O3+Y2O3)陶瓷层和次表层AlYMoSi合金层,所述的表层和次表层依次交替排列形成所述的多层结构涂层,所述的多层结构涂层通过AlYMoSi合金层与基体γ‑TiAl合金表面连接,其步骤为:采用磁控溅射技术,通过分别对(Al2O3+Y2O3)靶材和AlYMoSi靶材交替进行溅射,通过对工作气压、溅射功率、以及靶材‑基体间距等工艺参数的调节与控制,在基体γ‑TiAl合金表面形成(Al2O3+Y2O3)/AlYMoSi多层结构涂层。该方法效率高、工艺简单,且制备的(Al2O3+Y2O3)/AlYMoSi多层结构高温防护涂层结构致密、性能优良。
Description
技术领域
本发明涉及航空发动机零件表面防护技术领域,具体涉及一种γ-TiAl合金表面高温防护涂层的设计和方法。
背景技术
γ-TiAl合金具有高的高温屈服强度、高的蠕变抗力和断裂韧性,以及低的缺口敏感性,与传统的镍基高温合金相比,其比强度更高,是航空、航天飞行器理想的新型高温结构材料。然而在超过750℃的高温下,Ti-Al金属间化合物的抗氧化性能急剧下降。同时,由于高温下N、O原子渗入,合金易产生次表层脆化现象。因此,目前γ-TiAl合金的有效使用温度不能满足发动机热端部件的工作要求。
在正常氧化条件下,γ-TiAl合金的氧化膜主要组成相是TiO2和Al2O3。在所有氧化膜中,Al2O3是最具保护性的氧化物之一,化学稳定性高,而且氧离子在其中扩散系数很低。TiO2具有疏松的结构和较大的氧渗透率,在高温下难以赋予合金充分的抗氧化保护作用。Ti-Al金属间化合物中尽管含有大量的铝,但从热力学条件看,Al2O3和TiO2的生成自由能十分接近,而且铝的活度与其成分存在严重的负偏差,即使是含Al量最高的γ-TiAl合金,也很难通过铝的选择性氧化形成具有保护性的连续Al2O3氧化膜。
在保持γ-TiAl合金整体力学性能的前提下提高其抗高温氧化性能,最有效的方法便是在合金表面制备抗氧化性优良的保护涂层。然而,传统的硬质涂层易剥落,合金涂层在高温下长期服役时因互扩散而导致抗氧化性能快速下降,传统化学热处理易导致氢脆(如Surface and Coatings Engineering杂志1998年第110卷57-61页报道的研究结果)。
多层结构涂层增加了界面数,有利于阻碍氧元素向基体的内扩散,从而延长涂层的使用寿命,如:Corrosion Science杂志2014年第80卷19-27页报道的在8Nb-TiAl合金表面制备(Al2O3+Y2O3)/YSZ多层膜一文就提到了这一观点,然而(Al2O3+Y2O3)/YSZ多层膜在长时间高温服役的条件下易出现的裂纹扩散情况限制了其进一步的研发和应用。
为了尽快满足航空航天等领域对轻比重、高性能的高温结构材料的迫切需求,γ-TiAl合金的高温抗氧化性能的提高与解决已成为关键的工程问题之一。
发明内容
本发明目的是针对现有技术的不足,提供了一种具备一定自修复性能的(Al2O3+Y2O3)/AlYMoSi多层结构高温防护涂层,并提供其制备方法,以提高γ-TiAl合金的抗高温氧化性能。
实现本发明目的的技术解决方案是:一种在γ-TiAl合金表面制备的(Al2O3+Y2O3)/AlYMoSi多层结构涂层,包括表层(Al2O3+Y2O3)陶瓷层和次表层AlYMoSi合金层,所述的表层和次表层依次交替排列形成所述的多层结构涂层,所述的多层结构涂层通过AlYMoSi合金层与基体γ-TiAl合金表面连接。
其中,所述的(Al2O3+Y2O3)陶瓷厚度为2~5μm;所述的AlYMoSi合金层的厚度为1~3μm,所述的多层结构涂层的总厚度为50~80μm。
(Al2O3+Y2O3)陶瓷层的成分配比为:Al2O3占95~99wt%,余量为Y2O3。
AlYMoSi合金层的成分配比为:Al占45~50wt%,Mo占15~20wt%,Si占25~30wt%,Y占2~5wt%。
一种在γ-TiAl合金表面制备(Al2O3+Y2O3)/AlYMoSi多层结构涂层的方法,采用磁控溅射技术,将基体γ-TiAl合金置于工件台上,在溅射源上分别装上(Al2O3+Y2O3)靶材和AlYMoSi靶材,对基体γ-TiAl合金进行交替溅射镀膜处理,其中表层为(Al2O3+Y2O3)陶瓷层,次表层为AlYMoSi合金层,依次交替沉积,直至与基体γ-TiAl合金接触的沉积层为AlYMoSi合金层。其具体步骤如下:
1)将基体γ-TiAl合金与溅射靶材装入磁控溅射装置中,γ-TiAl合金置于试样台上,(Al2O3+Y2O3)陶瓷靶和AlYMoSi合金靶分别装入不同的溅射源枪套中;
2)抽真空,送入氩气,点击AlYMoSi合金靶溅射电源,调试工艺参数为:
溅射功率:150~200W;
工作气压:0.3~0.5Pa;
基体与靶材间距:20~35mm;
溅射时间:1h;
3)关闭AlYMoSi合金靶溅射电源,开启(Al2O3+Y2O3)陶瓷靶溅射电源,调试工艺参数为:
溅射功率:250~300W;
工作气压:0.3~0.5Pa;
基体与靶材间距:20~35mm;
溅射时间:2h;
4)依次交替沉积,直至涂层总厚度达到50~80μm。
与现有技术相比,本发明的有益效果在于:
1)多层结构涂层增加了界面数,有利于阻碍氧元素向基体的内扩散,从而延长涂层的使用寿命。
2)(Al2O3+Y2O3)/AlYMoSi多层结构涂层中的(Al2O3+Y2O3)表面功能防护层赋予γ-TiAl合金充分的抗氧化能力。
3)(Al2O3+Y2O3)/AlYMoSi多层结构涂层中的AlYMoSi自修复元素补给层中Mo、Si元素易聚集于涂层的裂纹处,能在高温条件下形成Mo与Si的氧化物以作为裂纹的“填充物”,将裂纹填补修补,因而克服在高温条件下(Al2O3+Y2O3)功能防护层分解严重的问题。
4)(Al2O3+Y2O3)/AlYMoSi多层结构涂层中的AlYMoSi自修复元素补给层与基体合金结合,可在高温下长时间有效延缓沉积层中Al、Y原子的丢失,确保(Al2O3+Y2O3)功能防护层抗氧化特性的有效性和持久性。
5)涂层采用磁控溅射技术制备,即通过分别对(Al2O3+Y2O3)靶材和AlYMoSi靶材交替进行溅射,通过工作气压、溅射功率、以及靶材-基体间距的调节与控制,在基体γ-TiAl合金表面形成(Al2O3+Y2O3)/AlYMoSi多层结构涂层。该方法效率高、工艺简单,且制备的(Al2O3+Y2O3)/AlYMoSi多层结构高温防护涂层结构致密、性能优良。
附图说明
图1为γ-TiAl合金表面(Al2O3+Y2O3)/AlYMoSi多层结构涂层示意图。
具体实施方式
下面结合实施例对本发明作进一步详细说明。但对于本领域技术人员来说,完全可以在具体实施方式所列数值的基础上进行合理的概括和推导。
实施例一:
1)将基体γ-TiAl合金与溅射靶材装入磁控溅射装置中,γ-TiAl合金置于试样台上,(Al2O3+Y2O3)陶瓷靶和AlYMoSi合金靶分别装入不同的溅射源枪套中。
2)抽真空,送入氩气,点击AlYMoSi合金靶溅射电源,调试工艺参数为:
溅射功率:200W
工作气压:0.4Pa
基体与靶材间距:20mm
溅射时间:1h
3)关闭AlYMoSi合金靶溅射电源,开启(Al2O3+Y2O3)陶瓷靶溅射电源,调试工艺参数为:
溅射功率:300W
工作气压:0.4Pa
基体与靶材间距:20mm
溅射时间:2h
4)依次交替循环8次。
5)关闭电源,破真空、取试样,完成(Al2O3+Y2O3)/AlYMoSi多层结构涂层的制备。
所制得(Al2O3+Y2O3)/AlYMoSi多层结构涂层其结构示意图如图1,制得的涂层均匀致密,无裂纹、孔洞等缺陷,其总厚度达到60μm,其中(Al2O3+Y2O3)陶瓷层厚5μm,AlYMoSi合金层厚3μm。在1000°C下高温氧化实验200h后,涂层依然保持完好、致密,未出现剥落、开裂等现象,其氧化增重值为4.3mg/cm2,较基体γ-TiAl合金的氧化增重值12.7mg/cm2有了明显的下降。
实施例二:
1)将基体γ-TiAl合金与溅射靶材装入磁控溅射装置中,γ-TiAl合金置于试样台上,(Al2O3+Y2O3)陶瓷靶和AlYMoSi合金靶分别装入不同的溅射源枪套中。
2)抽真空,送入氩气,点击AlYMoSi合金靶溅射电源,调试工艺参数为:
溅射功率:150W
工作气压:0.3Pa
基体与靶材间距:30mm
溅射时间:1h
3)关闭AlYMoSi合金靶溅射电源,开启(Al2O3+Y2O3)陶瓷靶溅射电源,调试工艺参数为:
溅射功率:250W
工作气压:0.3Pa
基体与靶材间距:30mm
溅射时间:2h
4)依次交替循环10次。
5)关闭电源,破真空、取试样,完成(Al2O3+Y2O3)/AlYMoSi多层结构涂层的制备。
所制得(Al2O3+Y2O3)/AlYMoSi多层结构涂层均匀致密,无裂纹、孔洞等缺陷,其总厚度达到50μm,其中(Al2O3+Y2O3)陶瓷层厚3μm,AlYMoSi合金层厚2μm。在1100°C下高温氧化实验100h后,涂层依然保持完好、致密,未出现剥落、开裂等现象,其氧化增重值为3.1mg/cm2,较基体γ-TiAl合金的氧化增重值8.5mg/cm2有了明显的下降。
本发明在γ-TiAl合金表面制备的多层结构高温防护涂层与一般的陶瓷或合金涂层不同,而是由AlYMoSi自修复元素补给层和(Al2O3+Y2O3)功能防护层组成。外层的(Al2O3+Y2O3)功能防护层赋予γ-TiAl合金充分的抗氧化能力;AlYMoSi自修复元素补给层与基体合金结合,可在高温下长时间有效延缓(Al2O3+Y2O3)功能防护层中Al、Y原子的丢失,确保(Al2O3+Y2O3)功能防护层抗氧化特性的有效性和持久性。并且AlYMoSi自修复元素补给层中Mo、Si元素易聚集于涂层的裂纹处,能在高温条件下形成Mo与Si的氧化物以作为裂纹的“填充物”,将裂纹填补修补,因而克服在高温条件下(Al2O3+Y2O3)功能防护层分解严重的问题。此外,多层结构涂层增加了界面数,有利于阻碍氧元素向基体的内扩散,从而延长涂层的使用寿命。通过本发明方法在γ-TiAl合金表面制备的(Al2O3+Y2O3)/AlYMoSi多层结构高温防护涂层可赋予其长期优良的抗高温氧化性能,同时基体材料的性能得以完整保留。由于研究对象的典型性,其研究成果将能推广到其它领域,其工程价值也非常突出。
Claims (8)
1.一种γ-TiAl合金表面Al2O3+Y2O3/AlYMoSi多层结构涂层,其特征在于,包括表层Al2O3+Y2O3陶瓷层和次表层AlYMoSi合金层,所述的表层和次表层依次交替排列形成所述的多层结构涂层,所述的多层结构涂层通过AlYMoSi合金层与基体γ-TiAl合金表面连接。
2.如权利要求1所述的多层结构涂层,其特征在于,Al2O3+Y2O3陶瓷层厚度为2~5μm。
3.如权利要求1所述的多层结构涂层,其特征在于,AlYMoSi合金层的厚度为1~3μm。
4.如权利要求1所述的多层结构涂层,其特征在于,多层结构涂层的总厚度为50~80μm。
5.如权利要求1所述的多层结构涂层,其特征在于,Al2O3+Y2O3陶瓷层的成分配比为:Al2O3占95~99wt%,余量为Y2O3。
6.如权利要求1所述的多层结构涂层,其特征在于,AlYMoSi合金层的成分配比为:Al占45~50wt%,Mo占15~20wt%,Si占25~30wt%,Y占2~5wt%。
7.一种如权利要求1-6任一所述的多层结构涂层的制备方法,其特征在于,采用磁控溅射技术,将基体γ-TiAl合金置于工件台上,在溅射源上分别装上Al2O3+Y2O3靶材和AlYMoSi靶材,对基体γ-TiAl合金进行交替溅射镀膜处理,其中表层为Al2O3+Y2O3陶瓷层,次表层为AlYMoSi合金层,依次交替沉积,直至达到所需厚度,且与基体γ-TiAl合金接触的沉积层为AlYMoSi合金层。
8.如权利要求7所述的制备方法,其特征在于,具体包括如下步骤:
1)将基体γ-TiAl合金与溅射靶材装入磁控溅射装置中,γ-TiAl合金置于试样台上,Al2O3+Y2O3陶瓷靶和AlYMoSi合金靶分别装入不同的溅射源枪套中;
2)抽真空,送入氩气,点击AlYMoSi合金靶溅射电源,调试工艺参数为:
溅射功率:150~200W;
工作气压:0.3~0.5Pa;
基体与靶材间距:20~35mm;
溅射时间:1h;
3)关闭AlYMoSi合金靶溅射电源,开启Al2O3+Y2O3陶瓷靶溅射电源,调试工艺参数为:
溅射功率:250~300W;
工作气压:0.3~0.5Pa;
基体与靶材间距:20~35mm;
溅射时间:2h;
4)依次交替沉积,直至涂层总厚度达到50~80μm。
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