改变定向凝固工艺参数抑制DZ22B合金与高纯Al2O3模壳面层的界面反应

刘雁焘 刘满平 孙少纯

刘雁焘, 刘满平, 孙少纯. 改变定向凝固工艺参数抑制DZ22B合金与高纯Al2O3模壳面层的界面反应[J]. 航空材料学报, 2020, 40(5): 60-69. doi: 10.11868/j.issn.1005-5053.2019.000174
引用本文: 刘雁焘, 刘满平, 孙少纯. 改变定向凝固工艺参数抑制DZ22B合金与高纯Al2O3模壳面层的界面反应[J]. 航空材料学报, 2020, 40(5): 60-69. doi: 10.11868/j.issn.1005-5053.2019.000174
Yantao LIU, Manping LIU, Shaochun SUN. Inhibition of interface reaction of DZ22B alloy and high purity Al2O3 mould surface by changing directional solidification process parameters[J]. Journal of Aeronautical Materials, 2020, 40(5): 60-69. doi: 10.11868/j.issn.1005-5053.2019.000174
Citation: Yantao LIU, Manping LIU, Shaochun SUN. Inhibition of interface reaction of DZ22B alloy and high purity Al2O3 mould surface by changing directional solidification process parameters[J]. Journal of Aeronautical Materials, 2020, 40(5): 60-69. doi: 10.11868/j.issn.1005-5053.2019.000174

改变定向凝固工艺参数抑制DZ22B合金与高纯Al2O3模壳面层的界面反应

doi: 10.11868/j.issn.1005-5053.2019.000174
详细信息
    通讯作者:

    刘满平(1964—),男,教授,主要从事铸造及铝合金大塑性变形研究,联系地址:江苏大学材料科学与工程学院,镇江(212013),E-mail:manpingliu@ujs.edu.cn

  • 中图分类号: Times new roman

Inhibition of interface reaction of DZ22B alloy and high purity Al2O3 mould surface by changing directional solidification process parameters

  • 摘要: 采用改变定向凝固工艺参数的方法研究浇注温度与抽拉速率对DZ22B镍基高温合金与高纯Al2O3陶瓷模壳面层材料间界面反应影响。利用SLM观察界面反应宏观的不同特征区域,使用配备有EDS的SEM分析研究合金-模壳界面反应处的微观结构及对界面反应产物元素种类进行定性分析,通过XRD与XPS对界面反应产物的相与元素价态进行鉴定。结果表明,界面反应产物主要为HfO2与Al1.98Cr0.02O3且沿定向凝固方向呈现区域分布,且在保证定向凝固合金组织的前提下,降低浇注温度、提高抽拉速率能够抑制延缓界面反应的发生。

     

  • 图  1  蜡棒组树图

    Figure  1.  Group tree pattern of wax rods

    图  2  不同工艺参数下带有粘砂层的定向凝固DZ22B试棒照片及试棒表面不同高度局部体式显微镜放大图 (a)浇注温度:1550 ℃,抽拉速率:4 mm•min–1;(b)浇注温度:1530 ℃,抽拉速率:4 mm•min–1;(c)浇注温度:1550 ℃,抽拉速率:5 mm•min–1;(d)浇注温度:1510 ℃,抽拉速率:6 mm•min–1

    Figure  2.  Photographs of directional solidification DZ22B test bar with sand layer under different process parameters and magnified image of local body microscope with different heights on the surface of test bar (a)pouring temperature:1550 ℃,withdrawal rate:4 mm•min–1;(b)pouring temperature:1530 ℃,withdrawal rate:4 mm•min–1;(c)pouring temperature:1550 ℃,withdrawal rate:5 mm•min–1;(d)pouring temperature:1510 ℃,withdrawal rate:6 mm•min–1

    图  3  未经腐蚀剂腐蚀试棒特征区域横截面的SEM微观结构图像 (a)region 2;(b)region 3

    Figure  3.  SEM microstructure images of the cross section of the characteristic area of the test bar without corrosion agent (a)region 2;(b)region 3

    图  4  经腐蚀剂腐蚀试棒特征区域横截面的SEM微观结构图像 (a)region 2;(b)region 3

    Figure  4.  SEM microstructure images of the cross section of the characteristic region of the test rod by corrosive agent(a)region 2;(b)region 3

    图  5  DZ22B合金界面反应特征区域region 2与region 3产物的XRD图谱

    Figure  5.  XRD pattern of the region 2 and region 3 products of the DZ22B alloy interface reaction characteristic region

    图  6  DZ22B合金界面反应特征区域region 2产物的XPS分析 (a)Hf;(b)O

    Figure  6.  XPS analysis of the DZ22B alloy interfacial reaction characteristic region products of the region 2 (a)Hf;(b)O

    图  7  DZ22B合金界面反应特征区域region 3产物的XPS分析 (a)Cr;(b)Al;(c)O

    Figure  7.  XPS analysis of the DZ22B alloy interfacial reaction characteristic region products of the region 3 (a)Cr;(b)Al;(c)O

    图  8  不同定向凝固工艺参数条件下DZ22B合金定向凝固试棒横截面枝晶形貌

    Figure  8.  Cross-section dendritic morphologies of DZ22B alloy directional solidification test bar under different directional solidification process parameters

    表  1  DZ22B高温合金的化学成分(质量分数/%)

    Table  1.   Chemical composition of DZ22B superalloy(mass fraction/%)

    CCrCoWNbTiAlHfBNi
    0.1709.2009.30010.1000.9001.9005.2001.1600.016Bal.
    下载: 导出CSV

    表  2  熔融氧化铝粉末的化学成分(质量分数/%)

    Table  2.   Chemical composition of fused alumina powder(mass fraction/%)

    Al2O3Na2OSiO2Fe2O3
    99.740.230.010.02
    下载: 导出CSV

    表  3  陶瓷模壳的面层、过渡层及背层浆料的成分

    Table  3.   Composition of the surface layer,transition layer and backup layer slurry of the ceramic mold shell

    SlurryMaterialComposition(mass fraction/%)
    Primary slurryRefractory:325 mesh fused aluminaRefractory loading(76%)
    Liquids:silica sol,wetting agent,defoamer and high purity deionized water Total liquids(24%)
    Transition slurryRefractory:220 mesh fused aluminaRefractory loading(70%)
    Liquids:silica sol,wetting agent,defoamer and high purity deionized water Total liquids(30%)
    Backup slurry Refractory:200 mesh fused alumina Tefractory loading(65%)
    Liquids:silica sol,wetting agent,defoamer and high purity deionized waterTotal liquids(35%)
    下载: 导出CSV

    表  4  4组模组对应的定向凝固工艺参数

    Table  4.   Directional solidification process parameters corresponding to the 4 groups of modules

    ModulePouring temperature/℃Withdrawal rate/mm•min–1
    115504
    215304
    315505
    415106
    下载: 导出CSV

    表  5  图3(a)中界面反应层与粘砂层的EDS分析结果(原子分数/ %)

    Table  5.   EDS analysis results of interface reaction layer and sand layer in Fig. 3(a)(atom fraction/%)

    LayerOAlSiHfCr
    Interfacial reaction layer61.6834.573.560.170.02
    Sand burning layer66.5230.063.42
    下载: 导出CSV

    表  6  图3(b)中界面反应层与粘砂层的EDS分析结果(原子分数/ %)

    Table  6.   EDS analysis results of interface reaction layer and sand layer in Fig. 3(atom fraction/%)

    LayerOAlSiHfCr
    Interfacial reaction layer60.7635.093.670.120.36
    Sand burning layer65.2331.263.390.12
    下载: 导出CSV

    表  7  图4(a)中界面反应层与粘砂层的EDS分析结果(原子分数/ %)

    Table  7.   EDS analysis results of interface reaction layer and sand layer in Fig. 4(a)(atom fraction/%)

    PositionCoOWHfTiCrAlNiSi
    19.11 3.503.570.292.4211.24 9.9659.91
    261.932.04 0.5939.77
    341.251.40 0.3548.3113.33
    下载: 导出CSV

    表  8  图4(b)中界面反应层与粘砂层的EDS分析结果(原子分数/ %)

    Table  8.   EDS analysis results of interface reaction layer and sand layer in Fig. 4(b)(atom fraction/%)

    PositionCoOWHfTiCrAlNiSi
    145.452.3114.4724.6213.15
    257.590.89 6.2116.1614.81
    39.15 3.493.610.232.52 9.6512.4358.92
    下载: 导出CSV

    表  9  与先前研究相比HfO2,Cr2O3和Al2O3的XPS峰的数值数据

    Table  9.   Numerical data of XPS peaks of HfO2,Cr2O3 and Al2O3 compared with previous studies

    Reaction productElementBinding energy/eVRef.
    This workLiterature data
    HfO2Hf 4f7/2/Hf 4f5/216.8/18.216.7/18.2[27]
    O 1s530.1530.2
    Al1.98Cr0.02O3Al 2p3/2/Al 2p1/273.873.5[2829]
    Cr 2p3/2/Cr 2p1/2576.7/586.5576.6/586.5
    O 1s530.6530.4
    下载: 导出CSV
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  • 收稿日期:  2019-11-25
  • 修回日期:  2020-09-15
  • 网络出版日期:  2020-09-10
  • 刊出日期:  2020-10-01

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