镍基高温合金<strong>K417G</strong>与氧化物耐火材料的界面反应

doi:10.11900/0412.1961.2021.00048

金属学报

2022, Vol. 58

Issue (7): 868-882 DOI: 10.11900/0412.1961.2021.00048

研究论文

本期目录 | 过刊浏览

镍基高温合金K417G与氧化物耐火材料的界面反应

宋庆忠¹^,², 潜坤¹^,³, 舒磊¹^,³, 陈波¹^,³(

), 马颖澈¹^,³, 刘奎¹^,³

^1.中国科学院金属研究所沈阳 110016
^2.东北大学冶金学院沈阳 110819
^3.中国科学院金属研究所师昌绪先进材料创新中心沈阳 110016

Interfacial Reaction Between Nickel-Based Superalloy K417G and Oxide Refractories

SONG Qingzhong¹^,², QIAN Kun¹^,³, SHU Lei¹^,³, CHEN Bo¹^,³(

), MA Yingche¹^,³, LIU Kui¹^,³

^1.Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
^2.School of Metallurgy, Northeastern University, Shenyang 110819, China
^3.Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

引用本文:

宋庆忠, 潜坤, 舒磊, 陈波, 马颖澈, 刘奎. 镍基高温合金K417G与氧化物耐火材料的界面反应[J]. 金属学报, 2022, 58(7): 868-882.
Qingzhong SONG, Kun QIAN, Lei SHU, Bo CHEN, Yingche MA, Kui LIU. Interfacial Reaction Between Nickel-Based Superalloy K417G and Oxide Refractories[J]. Acta Metall Sin, 2022, 58(7): 868-882.

全文: PDF(5547 KB) HTML

摘要:

研究了1600℃温度下Al₂O₃、CaO、MgO、Y₂O₃稳定ZrO₂、CaO稳定ZrO₂和Y₂O₃共6种材料坩埚与镍基高温合金K417G熔体的界面反应。结果表明：熔体对Al₂O₃坩埚以物理侵蚀为主,但坩埚易剥落导致合金中含有Al₂O₃夹杂物；CaO坩埚与合金界面处生成了液相Ca₃Al₂O₆,促进熔体与CaO之间的润湿性,导致界面处粘连严重；MgO坩埚与熔体中Al反应生成MgAl₂O₄并进入合金生成夹杂物；Y₂O₃稳定ZrO₂坩埚与合金界面处生成Al₂O₃反应层,但是Al₂O₃层未对坩埚发生侵蚀,可见这种坩埚具有较强的抗Al₂O₃渣的能力；CaO稳定ZrO₂坩埚与合金界面处生成液相CaAl₂O₄,导致坩埚失稳,向合金内剥落溶解；Y₂O₃坩埚与合金界面处主要生成Al₂Y₄O₉反应层,并且Y₂O₃向合金内溶解较为严重。坩埚和熔体交互作用对K417G熔体杂质O含量有显著影响,CaO、Y₂O₃和Y₂O₃稳定ZrO₂坩埚熔炼合金中O含量没有增加,而CaO稳定ZrO₂坩埚熔炼后O含量由0.0007% (质量分数)增加至0.0011%,MgO和Al₂O₃坩埚熔炼后,合金O含量增加明显,由0.0007%分别增加至0.0034%和0.0135%。

关键词 ：界面反应, K417G, 耐火材料, Al₂O₃, CaO, MgO, ZrO₂, Y₂O₃

Abstract：

High-performance nickel-based superalloys are highly desired in the aerospace industry. A drawback of vacuum induction melting for processing nickel-based superalloys is that oxide refractories contaminate the molten alloy through crucible-melt interaction. Therefore, crucibles used for producing nickel-based superalloys should be carefully selected to avoid melt contamination. In this study, the interfacial reaction between a molten nickel-based superalloy (K417G) and various oxide refractories, including Al₂O₃, CaO, MgO, ZrO₂ + 12%Y₂O₃ (mass fraction) (Y-PSZ), ZrO₂ + 20%CaO (CSZ), and Y₂O₃, formed by cold isostatic pressing was investigated at 1600^oC by XRD, SEM, and EDS. The effects of the oxide crucibles on the impurity contents of K417G were also evaluated. The results show that physical erosion is the primary mechanism of the interaction between Al₂O₃ crucibles and alloy melt. The readily detached Al₂O₃ particles formed inclusions in the alloy. The Ca₃Al₂O₆ liquid phase generated at the melt-crucible interface promoted wettability between the alloy and CaO crucible, resulting in a high adhesion at the interface. The reaction of the MgO crucible with Al in the alloy resulted in the formation of MgAl₂O₄ at the melt-crucible interface, which subsequently entered the alloy to form inclusions. Al₂O₃ was generated at the Y-PSZ-crucible-alloy interface. However, there was no corrosion of Al₂O₃in the Y-PSZ crucible, indicating the crucible exhibits excellent corrosion resistance to Al₂O₃ slags. The interaction between the CSZ crucible and alloy melt generated a CaAl₂O₄ liquid phase, making the crucible unstable to dissolve into the alloy. An Al₂Y₄O₉ reaction layer is mainly formed at the Y₂O₃-crucible-alloy interface. The dissolution of Y₂O₃ into the alloy melt was high compared to that of other oxide refractories. The melt-crucible interaction also significantly affected the oxygen content of K417G. The oxygen concentration of the alloy fused by CaO, Y₂O₃, and Y-PSZ crucibles did not increase, whereas that of the alloy melted in CSZ, MgO, and Al₂O₃ crucibles increased from 0.0007% to 0.0011%, 0.0034%, and 0.0135%, respectively.

Key words： interfacial reaction K417G refractory Al₂O₃ CaO MgO ZrO₂ Y₂O₃

收稿日期: 2021-01-26

ZTFLH:

TG146.1

作者简介: 宋庆忠,男,1996年生,硕士

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Raw material	Purity / (mass fraction, %)
Al₂O₃	≥ 99.61, MgO ≤ 0.10, SiO₂ ≤ 0.13, CaO ≤ 0.16, Fe₂O₃ ≤ 0.002, TiO₂ ≤ 0.01, Na₂O ≤ 0.03
CaO	≥ 96.78, MgO ≤ 0.53, Al₂O₃ ≤ 0.20, SiO₂ ≤ 0.05, TFe ≤ 0.01, TiO₂ ≤ 0.014, S ≤ 0.001, Loss ≤ 2.01
MgO	≥ 98.5, Fe ≤ 0.005, Ba ≤ 0.003, Cl^- ≤ 0.07, SO $4 2 -$ ≤0.05, Pb ≤ 0.005, Loss ≤ 4.5,
Y₂O₃	≥ 99.99, Loss ≤ 0.01
ZrO₂	≥ 99.0, Fe₂O₃ ≤ 0.005, MgO ≤ 0.05, CaO ≤ 0.05, TiO₂ ≤ 0.005, SiO₂ ≤ 0.01, Loss ≤ 1

表1 制作氧化物坩埚的原料纯度

表2 坩埚制作工艺参数、显气孔率和体积密度

图1 实验设备示意图

图2 不同氧化物坩埚的XRD谱

图3 Al2O3熔炼后K417G合金宏观形貌

图4 Al2O3坩埚熔炼后合金液面处的Al2O3夹杂物

图5 Al2O3坩埚与镍基高温合金K417G界面的SEM像及EDS元素分布图

表3 图5a中Al2O3坩埚与K417G合金界面处EDS分析结果 (atomic fraction / %)

图6 CaO坩埚与镍基高温合金K417G界面的SEM像及EDS元素分布图

表4 图6d中CaO坩埚与K417G合金界面处EDS分析结果 (atomic fraction / %)

图7 CaO熔炼的镍基高温合金K417G宏观形貌

图8 MgO坩埚与镍基高温合金K417G界面SEM像及EDS元素分布图

表5 图8a中MgO坩埚与K417G合金界面处EDS分析结果 (atomic fraction / %)

图9 MgO坩埚熔体上表面液面处镁铝尖晶石夹杂物

图10 Y2O3部分稳定的ZrO2 (Y-PSZ)坩埚与镍基高温合金K417G界面的SEM像及EDS元素分布图

表6 图10a中Y-PSZ坩埚与K417G合金界面处EDS分析结果 (atomic fraction / %)

图11 Y-PSZ坩埚熔炼后合金液面处的Al2O3夹杂物

图12 CaO完全稳定的ZrO2 (CSZ)坩埚与镍基高温合金K417G界面SEM像及EDS元素分布图

表7 CSZ坩埚与K417G合金界面处EDS分析结果(见图12~14各点) (atomic fraction / %)

图13 熔炼K417G合金后的CSZ坩埚背散射电子(BSE)像及EDS元素分布图

图14 CSZ坩埚原始形貌BSE像

图15 CSZ坩埚熔炼的K417G镍基高温合金宏观形貌

图16 Y2O3坩埚与镍基高温合金K417G界面SEM像及EDS元素分布图

图17 Y2O3坩埚与K417G合金界面组织及Y2O3坩埚熔炼后的K417G合金的BSE像

表8 图17a中Y2O3坩埚与K417G合金界面处EDS分析结果 (atomic fraction / %)

表9 熔炼后K417G合金内杂质元素含量 (atomic fraction / %)

图18 氧化物耐火材料的标准生成Gibbs自由能(ΔGθ )与温度的关系

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