CN110306216B - 一种活性元素Re改性β-(Ni,Pt)-Al涂层及其制备工艺 - Google Patents
一种活性元素Re改性β-(Ni,Pt)-Al涂层及其制备工艺 Download PDFInfo
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
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Abstract
本发明公开了一种活性元素Re改性β‑(Ni,Pt)‑Al涂层及其制备工艺,属于高温防护涂层技术领域。通过两次电镀加电弧离子镀的工艺,在Ni基单晶高温合金上制备Re改性β‑(Ni,Pt)‑Al涂层。包括以下步骤:在基体上电镀沉积Pt层;对电镀Pt层进行真空退火处理;电镀Ni‑Re层;在获得的Ni‑Re层上使用电弧离子镀沉积Al层;对获得的Al层在真空退火炉中退火获得Re改性β‑(Ni,Pt)‑Al涂层。本发明的优点:制备工艺简单,成本低;采用两次电镀的方法分别将Pt元素和Re元素加入到涂层中;涂层中的Re、Pt和Al元素含量以及涂层的厚度可精确的控制。
Description
技术领域
本发明涉及在高温合金基体上制备高温防护涂层的技术领域,具体涉及一种活性元素Re改性β-(Ni,Pt)-Al涂层及其制备工艺。
背景技术
高温合金由于其具有优异的力学和抗高温蠕变性能,因此被广泛应用作航空航天工业的热端件材料。为了不断提高燃气轮机发动机的工作效率,先进燃气轮机的进气温度可达1600℃,叶片工作温度可达1000~1200℃。由于叶片工作温度最高,同时受力复杂,新型发动机转子叶片采用了耐热温度更高的镍基单晶高温合金作为结构材料。为了保护这些关键热端部件并延长发动机热端部件的可靠服役寿命,一般均需在叶片表面涂覆高温防护涂层以保护基体合金不受高温氧化和热腐蚀的加速破坏。
热障涂层(TBCs)具有较低的热导率,TBCs施加到高温合金表面能起到隔热的作用,可使高温合金基体的表面温度降低100-300℃。但是,由于TBCs和高温合金之间的热膨胀系数相差较大和TBCs不能保护基体受高温氧化和热腐蚀的影响,因此需要在TBCs和高温合金基体之间添加连接层来解决这些问题。MCrAlY涂层和铝化物涂层常用来作为连接层。
简单铝化物涂层在高温氧化过程中生成致密而牢固的Al2O3膜,可有效阻碍高温氧化的继续进行,具有优良的抗氧化性能。但其氧化膜易剥落,抗长期氧化性能和抗热腐蚀能力欠佳。因此,在简单铝化物涂层中添加Cr,Si,Pt,Y和Re等活性元素,制备改性铝化物涂层,可以显著提高涂层的抗氧化和热腐蚀能力。
制备β-(Ni,Pt)-Al涂层,常用的方法是电镀Pt后采用CVD法气相渗铝。但是,由于Pt含量过高,在涂层的表面会形成PtAl2相,该相为脆性相,在服役过程中会恶化涂层的性能。所以,在气相渗铝前需加一步电镀层退火工艺,来稀释涂层表面Pt含量,可有效的避免PtAl2相的形成。另外,采用气相渗的方法,改性铝化物涂层的成分可控性较差。因此,研究新型β-(Ni,Pt)-Al涂层制备工艺,显得尤为重要。
在高温合金中加入Re可显著提高合金的使用温度,这是区别单晶高温合金代数产生的标志。鉴于Re在高温合金中的重要作用,将Re加入到MCrAlY涂层中也越来越受到人们的关注。发现,Re的加入对MCrAlY涂层的抗氧化性和热腐蚀能都有积极的影响。因此,本发明专利旨在,将Re元素加入到β-(Ni,Pt)-Al涂层中,并寻找一种制备一种Re改性的β-(Ni,Pt)-Al涂层制备方法。
发明内容
本发明目的是提供一种活性元素Re改性的β-(Ni,Pt)-Al涂层及其制备工艺,即运用两次电镀与电弧离子镀技术,制备出含Re的β-(Ni,Pt)-Al涂层,本发明工艺可有效地控制涂层中各种元素的含量,并且可以有效得避免涂层中PtAl2相的形成,从而提高涂层的抗氧化性能。
为实现上述目的,本发明所采用的技术方案如下:
一种活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,包括如下步骤:
(1)准备试样,并对试样进行预处理,预处理是指对试样依次进行电化学除油和活化处理;
(2)电镀纯Pt层:将试样置于镀Pt溶液中电镀纯Pt层;
(3)将经步骤(2)制备的镀有纯Pt层的试样在高温条件下进行除氢和扩散处理,具体过程为:先在200-400℃条件下保温1-5h进行除氢处理,再升温至950-1150℃条件下保温1-4h进行扩散处理,以稀释试样表层Pt含量;
(4)将经步骤(3)进行扩散处理后的试样进行Ni-Re复合电镀,以在涂层中引进元素Re,在试样表面的纯Pt层上形成Ni-Re层;
(5)在镀有Ni-Re层的试样上采用电弧离子镀沉积纯Al层;
(6)将步骤(5)中所得涂层进行退火处理,退火温度为950-1100℃,保温1-4h,即获得所述活性元素Re改性的β-(Ni,Pt)-Al涂层。
上述步骤(1)中,所述试样为镍基单晶高温合金;对试样进行预处理前,先对试样依次进行打磨、喷砂处理和超声清洗,具体过程为:首先,将试样使用SiC砂纸打磨至800#,并将试样圆角处进行倒角;然后将试样采用200目氧化铝丸进行湿喷砂处理;最后将试样依次在去离子水、酒精和丙酮中分别超声清洗20min。
上述步骤(1)中,所述电化学除油的具体工艺为:在5-15g/L的氢氧化钠溶液中进行电化学除油,基体作为阴极,不锈钢板作为阳极,在电流密度为2-15A/dm2下处理1-10min;所述活化工艺的过程为:将基体放入活化液中处理处理0.5-5min,所述活化液的组成为:盐酸为10-30vol.%,磷酸为5-25vol.%,其余为去离子水。
上述步骤(2)中,所述镀Pt溶液组成为:二亚硝基二氨铂5-15g/L,氨基磺酸30-55g/L,十二烷基硫酸钠0.05-0.1g/L,其余为水;电镀纯Pt层过程中:镀液pH为2-5,温度为50-95℃,在电流密度为0.5-4A/dm2下电镀20-120min,所获得的纯Pt层的厚度为1-10μm。
上述步骤(3)中,所述的除氢和扩散处理均在真空下进行,加热升温速率为5-10℃/min,随炉冷却。
上述步骤(4)中,电镀Ni-Re层之前,需先对扩散处理后的试样进行步骤(1)中的预处理过程(即电化学除油和活化工艺),以获得新鲜表面;进行Ni-Re复合电镀时,所用镀液组成为:KReO41×10-4-1×10-3mol/L,柠檬酸0.1-0.5mol/L,Ni2SO4·6H2O 0.1-0.5mol/L,其余为水;复合电镀过程中:使用氨水调节镀液pH为6-10,将电镀液加热到30-70℃,在电流密度为1-6A/dm2条件下电镀10-60min,所获得的Ni-Re层厚度为5-15μm。
上述步骤(5)中,所获得的纯Al层的厚度为10-50μm。
上述步骤(6)中,所述退火是在真空退火炉中进行的,升温速率为5-10℃/min,随炉冷却。
采用上述工艺在镍基单晶高温合金表面制备了活性元素Re改性的β-(Ni,Pt)-Al涂层,该涂层包括β-(Ni,Pt)-Al相和Re相,不含PtAl2相。
按重量百分含量计,该涂层化学成分为:Re 0.1-3wt.%,Al20-50wt.%,Pt 15-40wt.%,Ni 30-60wt.%。
本发明具有如下优点:
1、本发明采用两次电镀的方法首次将Re元素加入到β-(Ni,Pt)-Al涂层中。
2、本发明采用电镀加电弧离子镀结合的工艺,所制备的Re改性β-(Ni,Pt)-Al涂层为Re均匀分布于β-(Ni,Pt)-Al相中的结构。
3、本发明采用电镀的方法将Pt和Re这两种贵金属改性元素加入到涂层中,制备成本较低。
4、本发明采用电镀加电弧离子镀结合的方法制备了一种活性元素改性的β-(Ni,Pt)-Al涂层。涂层中的Re、Pt和Al元素以及涂层的厚度可精确的控制。涂层中没有任何杂质的引入。
附图说明
图1为涂层退火后的XRD图谱分析。
图2为退火后的Re改性β-(Ni,Pt)-Al涂层的截面形貌。
图3为Re改性β-(Ni,Pt)-Al涂层和β-(Ni,Pt)-Al涂层1200℃恒温氧化动力学曲线。
具体实施方式
以下结合附图及实施例详述本发明。
实施例1
基体采用一种单晶高温合金,其成分如下(质量百分比):Cr:8.0,Co:10.0,W:11.0,Al:6.0,Nb:1.5,Ti:1.0,Mo:1.0,C:0.1,B:0.01,Ni:余量。使用线切割将高温合金棒沿(001)方向切割成直径为18mm厚度为2mm的圆片。并在试样距边缘1mm处加工一个直径为2mm的圆孔,以方便电镀和电弧离子镀过程中悬挂式样。
对试样进行表面处理。使用SiC砂纸将式样打磨至800#,并将试样圆角处进行倒角。再将试样采用200#氧化铝丸进行湿喷砂处理,最后将试样依次在去离子水,酒精和丙酮中分别超声清洗20min。
对所有的试样进行预处理。电化学除油具体工艺:在10g/L的氢氧化钠溶液中进行电化学除油,基体作为阴极,不锈钢板作为阳极,在电流密度为5A/dm2下处理6min。所述的活化工艺为:将基体放入体积分数为30%的盐酸和5%磷酸,其余为去离子水的溶液中处理5min。以获得新鲜表面。
将预处理后的试样放入电镀液进行电镀Pt。镀液的成分为:6g/L的的二亚硝基二氨铂,50g/L氨基磺酸,0.1g/L的十二烷基硫酸钠,其余为水。电镀Pt工艺为:镀液pH为5,温度为95℃,在电流密度为3.5A/dm2下电镀60min。
将施加Pt层的试样在真空退火炉中加热到400℃并保温2h。随后继续加热至1000℃保温2h进行扩散处理。此过程加热速率为10℃/min,随炉冷却。
对在电镀Pt退火后的试样重复上述的预处理,然后进行电镀Ni-Re。所述的电镀Ni-Re层镀液成分为:1×10-4mol/L KReO4,0.4mol/L柠檬酸和0.5mol/L的Ni2SO4·6H2O,其余为水。电镀工艺为:使用氨水调节PH为7,将电镀液加热到35℃,在电流密度为5.5A/dm2下电镀45min,所获得的Ni-Re层厚度约为15μm。
采用电弧离子镀技术,在电镀Ni-Re后的试样上沉积Al层。Al层的厚度约为30μm。详细电弧离子镀工艺见表1。
表1电弧离子镀沉积Al层工艺
将沉积Al层的试样放入真空退火炉中,加热到1080℃保温5h后,随炉冷却。加热速率为10℃/min。
在本实施例中。由图1的XRD图谱分析可知,涂层退火后,主要为β-(Ni,Pt)-Al相,不含有PtAl2相。由于Re的加入,也可以发现Re的衍射峰。
图2为涂层退火后的扫面电镜截面背散射形貌图。可以看出,整个涂层的厚度约为50μm。由于Re在β相中极低的固溶度,结合EDS分析,涂层外层的白色析出相都为Re。涂层中Re含量为0.5wt.%,Al元素的含量为22wt.%,Pt元素含量为16wt.%,其余为Ni。
图3为Re改性PtAl涂层和普通PtAl涂层1200℃恒温氧化动力学曲线。可以看出,由于Re的加入,在氧化110h后涂层的总增重明显小于普通PtAl涂层。表明,Re的加入可以降低涂层的氧化速率,从而可以延长涂层的使用寿命。
Claims (10)
1.一种活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:该工艺包括如下步骤:
(1)准备试样,并对试样进行预处理,预处理是指对试样依次进行电化学除油和活化处理;
(2)电镀纯Pt层:将试样置于镀Pt溶液中电镀纯Pt层;
(3)将经步骤(2)制备的镀有纯Pt层的试样在高温条件下进行除氢和扩散处理,具体过程为:先在200-400℃条件下保温1-5h进行除氢处理,再升温至950-1150℃条件下保温1-4h进行扩散处理,以稀释试样表层Pt含量;
(4)将经步骤(3)进行扩散处理后的试样进行Ni-Re复合电镀,以在涂层中引进元素Re,在试样表面的纯Pt层上形成Ni-Re层;进行Ni-Re复合电镀时,所用镀液组成为:KReO4 1×10-4-1×10-3mol/L,柠檬酸0.1-0.5mol/L,Ni2SO4·6H2O 0.1-0.5mol/L,其余为水;复合电镀过程中:使用氨水调节镀液pH为6-10,将电镀液加热到30-70℃,在电流密度为1-6A/dm2条件下电镀10-60min,所获得的Ni-Re层厚度为5-15μm;
(5)在镀有Ni-Re层的试样上采用电弧离子镀沉积纯Al层;
(6)将步骤(5)中所得涂层进行退火处理,退火温度为950-1100℃,保温1-4h,即获得所述活性元素Re改性的β-(Ni,Pt)-Al涂层。
2.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(1)中,所述试样为镍基单晶高温合金;对试样进行预处理前,先对试样依次进行打磨、喷砂处理和超声清洗,具体过程为:首先,将试样使用SiC砂纸打磨至800#,并将试样圆角处进行倒角;然后将试样采用200目氧化铝丸进行湿喷砂处理;最后将试样依次在去离子水、酒精和丙酮中分别超声清洗20min。
3.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(1)中,所述电化学除油的具体工艺为:在5-15g/L的氢氧化钠溶液中进行电化学除油,基体作为阴极,不锈钢板作为阳极,在电流密度为2-15A/dm2下处理1-10min;所述活化工艺的过程为:将基体放入活化液中处理处理0.5-5min,所述活化液的组成为:盐酸为10-30vol.%,磷酸为5-25vol.%,其余为去离子水。
4.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(2)中,所述镀Pt溶液组成为:二亚硝基二氨铂5-15g/L,氨基磺酸30-55g/L,十二烷基硫酸钠0.05-0.1g/L,其余为水;电镀纯Pt层过程中:镀液pH为2-5,温度为50-95℃,在电流密度为0.5-4A/dm2下电镀20-120min,所获得的纯Pt层的厚度为1-10μm。
5.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(3)中,所述的除氢和扩散处理均在真空下进行,加热升温速率为5-10℃/min,随炉冷却。
6.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(4)中,电镀Ni-Re层之前,需先对扩散处理后的试样进行步骤(1)中的预处理过程,以获得新鲜表面。
7.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(5)中,所获得的纯Al层的厚度为10-50μm。
8.根据权利要求1所述活性元素Re改性的β-(Ni,Pt)-Al涂层的制备工艺,其特征在于:步骤(6)中,所述退火是在真空退火炉中进行的,升温速率为5-10℃/min,随炉冷却。
9.一种利用权利要求1-8任一所述方法制备的活性元素Re改性的β-(Ni,Pt)-Al涂层,其特征在于:该涂层制备于镍基单晶高温合金表面,按重量百分含量计,该涂层化学成分为:Re 0.1-3wt.%,Al 20-50wt.%,Pt 15-40wt.%,Ni 30-60wt.%。
10.根据权利要求9所述的活性元素Re改性的β-(Ni,Pt)-Al涂层,其特征在于:该涂层包括β-(Ni,Pt)-Al相和Re相,Re均匀分布于β-(Ni,Pt)-Al相中;该涂层中不含PtAl2相。
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