Inhibition of interface reaction of DZ22B alloy and high purity Al2O3 mould surface by changing directional solidification process parameters
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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。Abstract: The effect of casting temperature and withdrawal rate on the interfacial reaction between DZ22B nickel-base superalloy and high-purity Al2O3 ceramic shell facecoat material was studied by changing the parameters of directional solidification process.The SLM was used to observe the different characteristic regions of the macroscopic reaction. The SEM analysis equipped with EDS was used to study the microstructure of the alloy-formed shell interface and the qualitative analysis of the interfacial reaction product elements. The phase and element valence of the interfacial reaction product were identified by XRD and XPS.The results show that the interface reaction products are mainly HfO2 and Al1.98Cr0.02O3 and exhibit a sub-regional distribution along the direction of directional solidification.Under the premise of ensuring the directionally solidified alloy structure, lowering the pouring temperature and increasing the withdrawal rate can inhibit the occurrence of delayed interface reaction.
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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/%）
C Cr Co W Nb Ti Al Hf B Ni 0.170 9.200 9.300 10.100 0.900 1.900 5.200 1.160 0.016 Bal. 
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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/%）
Al2O3 Na2O SiO2 Fe2O3 99.74 0.23 0.01 0.02
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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
Slurry Material Composition（mass fraction/%） Primary slurry Refractory：325 mesh fused alumina Refractory loading（76%） Liquids：silica sol，wetting agent，defoamer and high purity deionized water Total liquids（24%） Transition slurry Refractory：220 mesh fused alumina Refractory 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 water Total liquids（35%）
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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
Module Pouring temperature/℃ Withdrawal rate/mm•min–1 1 1550 4 2 1530 4 3 1550 5 4 1510 6
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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/%）
Layer O Al Si Hf Cr Interfacial reaction layer 61.68 34.57 3.56 0.17 0.02 Sand burning layer 66.52 30.06 3.42 — —
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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/%）
Layer O Al Si Hf Cr Interfacial reaction layer 60.76 35.09 3.67 0.12 0.36 Sand burning layer 65.23 31.26 3.39 — 0.12
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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/%）
Position Co O W Hf Ti Cr Al Ni Si 1 9.11 3.50 3.57 0.29 2.42 11.24 9.96 59.91 — 2 — 61.93 — 2.04 — 0.59 39.77 — — 3 — 41.25 — 1.40 — 0.35 48.31 — 13.33
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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/%）
Position Co O W Hf Ti Cr Al Ni Si 1 — 45.45 — 2.31 — 14.47 24.62 — 13.15 2 — 57.59 — 0.89 — 6.21 16.16 — 14.81 3 9.15 3.49 3.61 0.23 2.52 9.65 12.43 58.92 —
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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
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