Microstructure and properties of CoCrFeNiSix high-entropy alloy coating by laser cladding
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摘要: 为了探究Si元素含量对CoCrFeNiSix(x=0.5,1.0,1.5)高熵合金涂层的组织与性能的影响,采用激光熔覆技术制备高熵合金涂层,通过X射线衍射仪、扫描电子显微镜、能谱仪、显微硬度仪、摩擦磨损试验机、电化学工作站等表征了涂层的物相组成、微观组织以及元素分布、硬度值、耐磨性能和耐腐蚀性能. 研究表明,随着Si元素的含量增加,合金物相由单相面心立方结构转变为面心立方结构、Si元素化合物(σ)相结构,最后形成面心立方结构、体心立方结构和σ相混合结构.涂层的组织主要由柱状晶转变成树枝晶,最后形成胞状晶;同时,涂层的硬度不断提高,当Si含量为1.5时,涂层的平均硬度值达到最高,为619.04 HV0.2,约为基体的2.67倍.涂层的磨损量、摩擦系数随着Si含量的增加而减少,耐磨性能显著提高.涂层在3.5%NaCl溶液中腐蚀性能随着Si含量的增加先增加后降低,当Si含量为1.0时,涂层的耐腐蚀性能最优.Abstract: In order to investigate the effect of Si content on the microstructure and properties of CoCrFeNiSix (x=0.5, 1.0, 1.5) high-entropy alloy coating, the high-entropy alloy coating was prepared by laser cladding technology. The phase composition, microstructure, element distribution, hardness value, wear resistance and corrosion properties of the coating were characterized by X-ray diffraction, scanning electron microscopy (SEM), energy dispersive spectroscopy, microhardness tester, friction and wear tester, and electrochemical workstation. The results show that with the increase of Si content, the alloy phase changes from single-phase face-centered cubic structure to face-centered cubic structure, silicon compound (σ) phase structure, and finally form face-centered cubic structure, body-centered cubic structure and σ mixed structure. The microstructure of the coating mainly changes from columnar crystals to dendritic crystals and finally to cellular crystals. At the same time, the hardness of the coating also increases. When the Si content is 1.5, the average hardness of the coating reaches 619.04 HV0.2, which is about 2.67 times that of the substrate. The wear amount and friction coefficient of the coating decreased with the increase of Si content, and the wear resistance of the coating increased significantly. In 3.5%NaCl solution, the corrosion performance of the coating increases first and then decreases with the increase of Si content. When Si content is 1.0, the corrosion performance of the coating is optimal.
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Keywords:
- laser cladding /
- high-entropy alloy coating /
- wear resistance /
- corrosion resistance
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0. 序言
轻质耐高温结构材料是近十年来材料学科的研究热点之一, 高温钛合金轻质高强和优越的高温性能使得其成为提高高温部件性能的优选材料之一. Ti60 合金是近α型高温钛合金, 具有优良的综合力学性能, 其服役温度可达600 ℃, 在高温下具有良好的热强性和热稳定性[1-3]. Ti700sr钛合金是由中国船舶重工集团公司第七二五研究所与洛阳双瑞精铸钛业有限公司共同研制的一种新型近α型高温钛合金.通过α相固溶强化来提升合金的蠕变性能,通过合金元素之间的相互作用,有效的控制初生α相、硅化物与α2相的尺寸和含量,使得合金具有良好的室温强度、蠕变强度和疲劳性能,可在600 ℃以上温度短时使用.通过两种材料的结合应用可以发挥各自的优势,实现可靠焊接成为亟需解决的问题.
目前高温钛合金的焊接方法主要包括钨极氩弧焊、激光焊、真空电子束焊等[3-11]. 其中真空电子束焊具有功率密度高,能量密度集中,焊缝宽度窄,深宽比大,焊接热影响区小等特点.同时在真空条件下焊接钛合金焊缝不会被空气污染,焊接冶金质量好,因此非常适合于钛及钛合金的焊接.
文中对Ti60板材和Ti700sr铸件进行电子束焊接,研究异种高温钛合金电子束焊接接头组织特征,分析接头的显微硬度分布规律和力学性能,为Ti60板材和Ti700sr铸件电子束焊接技术在结构焊接中发挥更好的作用,优化结构设计方案提供技术支持.
1. 试验材料与方法
1.1 试验材料
试验材料选用1.5 mm厚的Ti60板材和10 mm厚的Ti700sr铸件,其中Ti700sr铸件经过热等静压.母材的化学成分如表1所示.两种材料的显微组织如图1所示.其中Ti60板材主要由等轴状初生α相和少量的α + β相组成.Ti700sr铸件主要由网篮状的α相和少量的残余β相组成.
表 1 母材名义成分(质量百分数,%)Table 1. Chemical composition of base metal材料 Ti Al Sn Zr Mo Si Nd Ti60 余量 5.5 4.0 3.5 1.0 0.4 0.85 Ti700sr 余量 6.0 1.0 4.0 0.5 0.35 − 1.2 试验方法
Ti60板材规格为300 mm × 150 mm × 1.5 mm,焊接坡口为止口对接坡口,在Ti700sr铸件上加工出1.5 mm锁底对接台阶,两条焊缝之间间隔10 mm,接头形式示意图如图2所示,焊缝长度为300 mm.装配间隙为0 ~ 0.2 mm.
试验采用EBOCAM KS610-TWIN G600KM大功率高压电子束焊机进行焊接.焊前采用激光清洗设备对待焊接的Ti60板材和Ti700sr铸件装配端面进行清洗,去除表面氧化膜,然后用丙酮擦洗干净.电子束焊接工艺参数如表2所示.
表 2 电子束焊接工艺Table 2. Process parameters of electron beam welding焊接电压U/kV 工作距离L/mm 焊接电流I/mA 焊接速度v/(mm·min−1) 扫描波形 150 800 15 1 200 − 150 800 2 800 双圆形 焊接完成后,对该焊接接头进行X射线检测,未发现气孔、裂纹、未熔合等焊接缺陷,满足GJB 1718A—2005的射线探伤Ⅰ级合格要求.
沿垂直于焊缝方向采用线切割制备接头金相试样,尺寸为40 mm × 30 mm × 20 mm,试样经机械抛光后进行腐蚀(腐蚀溶剂为氢氟酸(10 mL) + 硝酸(15 mL) + 水(75 mL)),采用Observer.Z1m金相显微镜观察.在JEM-2100 透射电镜下对制备的焊接接头透射试样进行观测.
根据GB/T 4340.1—2009《金属材料维氏硬度试验第1部分:试验方法》标准,在VMH-I04显微硬度计上对焊接接头进行显微硬度测试,从一侧母材到另一侧母材,间隔0.5 mm,测量载荷200 g,加载时间10 s.按照GB/T 2651—2008《焊接接头拉伸试验方法》在万能试验机上对焊接接头进行室温、600和650 ℃高温拉伸性能测试试验.
2. 结果及分析
2.1 显微组织
电子束焊接时采用止口对接,焊缝由两侧Ti60和Ti700sr母材自熔后重新凝固形成.焊后接头形貌如图3所示,接头截面上宽下窄,呈“漏斗形”,焊缝区宽度约3 mm.其中焊缝上表面过渡圆滑,没有明显的咬边等焊接缺陷.Ti60和Ti700sr对接部分焊缝较宽,其中Ti60的热影响区宽度明显大于Ti700sr.Ti60的热影响区宽度约有2 mm,而Ti700sr热影响区宽度仅有0.7 mm左右;焊缝下部Ti700sr铸件部分焊缝较窄.
电子束焊接热输入小,接头焊缝区冷却速度极快,焊缝组织由熔化后初始凝固而成的粗大β相转变为细小的针状马氏体α′组织,呈现出网篮形态,如图4所示.
焊缝下部Ti700sr母材焊接熔化量较大,板材Ti60熔化量较小,因此焊缝中成分更接近于Ti700sr母材.由于合金在电子束焊接快速冷却后α稳定元素来不及析出,从而固溶在β相内,通过切边相变转化为马氏体如图4a, 4b所示.高温停留时间极短使得马氏体来不及长大,形成交织的网篮细针状马氏体,马氏体内部存在较多的位错,如图4c所示,这在一定程度上提高了焊缝的强度.由于高温停留时间短,冷却速度快,未见明显的析出物大量析出聚集,进而保证了焊缝高温性能.
Ti700sr侧熔合区组织形貌如图5所示.熔合区两侧组织形貌存在较大的差异,如图5a所示.其中Ti700sr母材侧α组织存在一定程度的长大,由于焊接速度快,高温停留时间极短,熔合区作为焊缝和热影响区的过渡,可以发现α相虽然增多,但是尺寸相比于焊缝较小,相比于母材较大,实现了组织的有效过渡,避免显微尺寸的巨大差异,降低了显微组织的尺寸梯度.对熔合区组织进行透射电镜观测,可以发现马氏体内部存在层错和孪晶,如图5b所示.这在一定程度上可以改善接头协调变形的能力,提升材料承载能力.
从图5a可以发现焊接热影响区域极窄,大致只有100 μm.对Ti700sr侧热影响区组织进行高倍组织观测,如图6所示,可以发现相比于母材网篮状的α相长大,只有极少量的残余β相.
Ti60侧熔合区组织相貌如图7所示.熔合区两侧组织形貌存在较大的差异,熔合区并不明显,如图7a所示,主要是由于焊缝中熔入的Ti700sr的成分较多,使得焊缝更加接近Ti700sr,因此焊缝和热影响区的差异较大,熔合区的宽度较窄,未能形成明显的组织过渡.对熔合区进行透射电镜观测,发现弥散相在α相内析出,呈聚集状排列析出分布于相内和相界,尺寸较小,在400 nm左右,如图7b所示.
对于Ti60合金而言,热影响区温度较低,包含熔点以下到860 ℃温度区间[12],其满足α相溶解条件,如图8a所示,初生α相体积分数降低,会造成热稳定性下降[13].同时冷却速度相对焊缝较慢,容易满足稀土相析出的热力学条件[14],稀土相开始逐渐出现,如图8b所示,富Nd稀土弥散相[14]沿晶体的晶界、亚晶界和位错线等处析出.而且随着距焊缝距离的增加,稀土析出相含量逐渐增大到峰值,之后迅速降低并消失.
2.2 力学性能
2.2.1 显微硬度
焊接接头显微硬度分布情况如图9所示,焊缝区显微硬度与Ti700sr母材相当,基本在360 HV左右.硬度最高点出现在Ti60侧热影响区,硬度最大值达到418 HV,Ti60母材自身的硬度在370 HV左右,和Ti700sr母材相当.
在快速冷却条件下焊缝组织发生马氏体转变,β相向细小针状α′相转变,而α′相具有高的位错密度和孪晶,细小针状α′组织的出现导致了大量的晶界产生,而焊缝作为两种材料的混合区,相比于Ti700sr成分,焊缝中的α稳定元素所占比例降低,β稳定元素所占比例增大,从而使得焊缝的显微硬度与Ti700sr母材相当.而Ti60热影响区由于富Nd稀土弥散相的析出,使得该区域的显微硬度得到了大幅的提升.
2.2.2 室温拉伸性能
焊接接头室温拉伸性能如表3所示.接头抗拉强度达到1 100 MPa以上.接头断裂于Ti60热影响区,这主要是由于热影响区稀土相析出,同时热影响区生成粗大的柱状晶,微观组织为脆硬针状马氏体,一定程度上降低焊接接头的韧性和塑性,在受力时不能协调变形,造成应力集中从而容易造成失效断裂.
表 3 接头室温拉伸性能Table 3. Tensile Properties of joints at room temperature编号 温度 抗拉强度Rm/MPa 断裂位置 1-3 常温 1 125 Ti60热影响区 1-3 常温 1 105 Ti60热影响区 1-3 常温 1 182 Ti60热影响区 2.2.3 高温拉伸性能
焊接接头高温拉伸性能如表4所示.接头600 和650 ℃均断裂在Ti60母材.其中接头600 ℃高温拉伸性能均值为695 MPa,650 ℃高温拉伸性能均值为587 MPa. 这是因为电子束焊缝区很窄,在高温外加载荷的作用下,Ti60母材区先于焊缝区发生塑性变形,并且由于其它位置高温强度较好,最先在Ti60母材部位失效断裂,拉伸断裂后试样呈现塑性变形,表现为明显的颈缩现象.
表 4 接头高温拉伸性能Table 4. Tensile properties of joints at high temperature编号 温度T/℃ 抗拉强Rm/MPa 断裂位置 1-3 600 700 Ti60母材 1-3 600 695 Ti60母材 1-3 600 690 Ti60母材 4-6 650 583 Ti60母材 4-6 650 592 Ti60母材 4-6 650 585 Ti60母材 3. 结论
(1) 通过电子束焊接1.5 mm厚的Ti60板材和10 mm厚的Ti700sr铸件锁底对接接头,可以获得无气孔、裂纹、未熔合等内部缺陷的优质接头,接头质量达到GJB 1718A—2005 I 级检测标准.
(2) 焊缝为网篮形态的细小针状马氏体组织,Ti700sr侧熔合区α相有所增多,但是尺寸处于焊缝和母材之间,马氏体内部存在层错和孪晶.Ti700sr侧热影响区相比于母材网篮状的α相长大,只有极少量的残余β相.Ti60侧熔合区组织发现富Nd稀土弥散相在相内析出.Ti60侧热影响区富Nd稀土弥散相沿晶体的晶界、亚晶界和位错线等处呈聚集状析出.
(3) 焊缝区显微硬度与Ti700sr母材相当,基本在360 HV左右.硬度最高点出现在Ti60侧热影响区,硬度最大值达到418 HV,Ti60母材自身的硬度在370 HV左右,和Ti700sr母材相当.
(4) 接头室温抗拉强度达到1 100 MPa以上,断裂于Ti60热影响区.接头600 ℃高温拉伸性能均值为695 MPa,650 ℃高温拉伸性能均值为587 MPa.接头600 和650 ℃均失效断裂在Ti60母材.
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图 10 基体和CoCrFeNiSix (x = 0.5, 1.0, 1.5)高熵合金涂层磨损形貌
Figure 10. Wear morphology of matrix and CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy coatings. (a) matrix; (b) matrix (high magnification); (c) CoCrFeNiSi0.5; (d) CoCrFeNiSi0.5 (high magnification); (e) CoCrFeNiSi1.0; (f) CoCrFeNiSi1.0 (high magnification); (g) CoCrFeNiSi1.5; (h) CoCrFeNiSi1.5 (high magnification)
图 13 基体和CoCrFeNiSix (x = 0.5,1.0,1.5)高熵合金涂层在3.5%NaCl溶液中电化学腐蚀形貌
Figure 13. Electrochemical corrosion morphology of substrate and CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy coating in 3.5%NaCl solution. (a) matrix; (b) matrix (high magnification); (c) CoCrFeNiSi0.5; (d) CoCrFeNiSi0.5 (high magnification); (e) CoCrFeNiSi1.0; (f) CoCrFeNiSi1.0 (high magnification); (g) CoCrFeNiSi1.5; (h) CoCrFeNiSi1.5 (high magnification)
表 1 试验工艺参数
Table 1 Experimental process parameters
激光功率
P/kW扫描速度
v/(mm·s−1)光斑直径
d/mm搭接率
η(%)1.1 6 2 50 表 2 CoCrFeNiSix (x = 0.5, 1.0, 1.5) 高熵合金涂层的价电子浓度
Table 2 Valence electron concentrations of CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy coatings
x 价电子浓度VEC 0.5 7.78 1.0 7.40 1.5 7.09 表 3 CoCrFeNiSix (x = 0.5, 1.0, 1.5)的EDS分析(原子分数, %)
Table 3 EDS analysis of CoCrFeNiSix (x = 0.5, 1.0, 1.5)
x值 区域 Co Cr Fe Ni Si 0.5 设计含量 22.22 22.22 22.22 22.22 11.10 A 20.86 22.83 27.62 17.37 11.32 B 18.11 22.56 22.51 20.84 15.98 1.0 设计含量 20 20 20 20 20 C 16.49 16.30 42.93 13.26 11.02 D 14.91 14.77 33.58 18.19 18.55 x = 1.5 设计含量 18.18 18.18 18.18 18.18 27.27 E 6.31 6.81 33.63 5.26 47.99 F 8.19 15.17 39.24 9.00 28.40 表 4 CoCrFeNiSix (x = 0.5,1.0,1.5)高熵合金磨损形貌EDS分析(原子分数,%)
Table 4 EDS analysis of wear morphology of CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy
x值 位置 Co Cr Fe Ni Si O 0.5 G 8.14 6.92 27.97 7.81 2.55 46.60 1.0 H 5.59 5.38 28.97 5.25 3.87 50.94 1.5 J 5.86 6.48 22.72 5.24 8.75 50.95 表 5 CoCrFeNiSix (x = 0.5,1.0,1.5)高熵合金涂层的电化学参数
Table 5 Electrochemical parameters of CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy coating
合金 腐蚀电位
Ecorr /mV自腐蚀电流密度
icorr /(10−2A·cm−2)基体 −1 042.180 32.8 CoCrFeNiSi0.5 −997.063 1.92 CoCrFeNiSi1.0 −955.391 1.39 CoCrFeNiSi1.5 −1 039.342 3.37 表 6 CoCrFeNiSix (x = 0.5,1.0,1.5)高熵合金涂层电化学阻抗拟合结果
Table 6 Electrochemical impedance fitting results of CoCrFeNiSix (x = 0.5, 1.0, 1.5) high-entropy alloy coating
合金 溶液电阻Rs /Ω 钝化膜电容CPE1 /10−6F 钝化膜电阻Rf /103Ω 涂层的电容CPE2 /10−6F 电荷转移电阻Rct /102Ω 基体 6.045 39.58 0.047 9 1.931 1.632 CoCrFeNiSi0.5 1.392 16.83 0.011 0 8.507 39.62 CoCrFeNiSi1.0 9.401 9.698 0.007 1 5.869 49.05 CoCrFeNiSi1.5 8.83 13.43 0.513 5 31.96 38.35 -
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