半导体制程设备铝合金涂层腐蚀失效行为研究进展

doi:10.12068/j.issn.1005-3026.2025.20240182

摘要/Abstract

摘要：

在半导体制程设备中，在高温、真空、强腐蚀气体及其等离子体耦合作用下，铝合金涂层极易发生失效.在氯基等离子体中，阳极氧化涂层极易被刻蚀去除，Y₂O₃涂层的刻蚀速率约为阳极氧化涂层的1/50；在氟基等离子体中，阳极氧化涂层和Y₂O₃涂层均存在氟化物层剥落导致的颗粒问题.通过调节电解液的成分/温度、制备纯铝层可提高阳极氧化涂层的耐蚀性能，提高Y₂O₃涂层的致密性同样可降低涂层的刻蚀速率，结合远程等离子体清洗技术，避免带电粒子轰击腔室材料，可显著减少反应腔室中颗粒的产生.在刻蚀和薄膜沉积过程中，腔室表面成分发生变化，进而改变等离子体状态，将引发多种工艺缺陷.

关键词: 半导体制程设备, 阳极氧化涂层, Y₂O₃涂层, 腐蚀失效行为, 卤素气体, 等离子体

Abstract:

In the semiconductor fabrication equipment， the coatings on aluminum alloy often fail due to the coupling effect of high-temperature， vacuum and aggressive gases， including their plasma. In the chlorine-based plasma， the anodized coating has a high etching rate， leading to rapid removal， while the etching rate of Y₂O₃ coatings is approximately one in 50 of that of the anodized coating. In the fluorine-based plasma， both the anodized coating and Y₂O₃ coatings experience particle contamination due to the fluoride layer peeling. The corrosion resistance of the anodized coating can be significantly enhanced by adjusting the composition and temperature of the electrolyte or depositing a pure aluminum layer on the aluminum alloy surface. Additionally， improving the density of Y₂O₃ coatings can reduce their etching rate. Combining these strategies with remote plasma cleaning techniques can minimize the impact of charged particles on chamber materials， significantly reducing particle contamination in the reaction chamber. During the etching and thin film deposition processes， changes in the chamber surface composition can alter the plasma state， leading to various process defects.

Key words: semiconductor fabrication equipment, anodized coating, Y₂O₃ coating, corrosion fatigue behavior, halogen gas, plasma

中图分类号:

TG 178

赵阳, 王宇航, 张涛, 王福会. 半导体制程设备铝合金涂层腐蚀失效行为研究进展[J]. 东北大学学报（自然科学版）, 2025, 46(3): 28-45.

Yang ZHAO, Yu-hang WANG, Tao ZHANG, Fu-hui WANG. Research Progress on the Corrosion Failure Behavior of Coatings on Aluminum Alloy for Semiconductor Fabrication Equipment[J]. Journal of Northeastern University(Natural Science), 2025, 46(3): 28-45.

图/表 29

图1 集成电路制造工艺流程图［4］

Fig. 1 Flow chart of the integrated circuit fabrication process［4］

图2 电感耦合等离子体刻蚀腔室示意图[8]（a）—腔室结构剖面；（b）—反应腔室的原子复合过程；（c）—晶圆表面的原子复合过程.

Fig. 2 Schematic of the inductively-coupled plasma etching chamber[8]

表1 湿法擦拭/清洗步骤[14-16]

Table 1 Wet wiping/cleaning procedures[14-16]

湿法擦拭流程

湿法清洗流程

1. 启动腔室清洁

2. 冷却腔室

3. 泄压开腔

4. 湿洁净布擦拭面板

5. 使用N₂干燥面板

6. 关闭腔室

7. 加热腔室

8. 腔室检漏

9. 刻蚀/沉积工艺验证

10. 恢复运行

1. 启动腔室清洁

2. 冷却腔室

3. 泄压开腔

4. 拆卸腔室部件

5. 在清洗溶液中浸泡腔室部件

6. 烘干腔室部件

7. 更换腔室部件

8. 关闭腔室

9. 加热腔室

10. 腔室检漏

11. 刻蚀/沉积工艺验证

12. 恢复运行

图3 多孔阳极氧化铝的截面示意图[17]

Fig. 3 Cross-sectional schematic of the porous anodized aluminum[17]

图4 加工1 800片晶圆后金属铝刻蚀腔室的宏观形貌[18]

Fig.4 Macro-morphology of the aluminum etching chamber after 1 800 wafer fabrications[18]

图5 不同位置阳极氧化涂层的刻蚀速率随BCl3流量的变化[18]

Fig. 5 Variations of the etching rate for the anodized coating with BCl3 gas flow at different positions[18]

图6 阳极氧化涂层腔室的宏观形貌（a）—洁净的阳极氧化涂层腔室；（b）—被AlF x 腐蚀产物覆盖的阳极氧化涂层腔室［17］.

Fig. 6 Macro-morphology of the anodized coating chamber[17]

图7 阳极氧化涂层开裂的截面形貌[17]

Fig. 7 Cross-sectional morphology of the cracked anodized coating17]

图8 阳极氧化涂层在不同温度下经历热循环测试后的表面形貌[16]（a）—120 ℃；（b）—160 ℃；（c）—200 ℃.

Fig. 8 Surface morphology of the anodized coating treated by thermal cycling tests at various temperatures[16]

图9 F自由基通过阳极氧化涂层的缺陷/裂纹与铝合金基体反应的截面示意图[17]（a）—F自由基穿过涂层；（b）—F自由基与基体反应生成氟化铝.

Fig. 9 Cross-sectional schematic illustrating fluorine radicals penetrating the defects/cracks in the anodized aluminum and reacting with the aluminum substrate[17]

图10 阳极氧化涂层的失效过程[17]（a）—裂纹萌生；（b）—裂纹处生成AlF x 腐蚀产物；（c）—AlF x 腐蚀产物大量堆积.

Fig. 10 Failure processes of the anodized coating[17]

图11 Al2O3试样化学成分的变化[42]注：（a）为清洗前的Al2O3试样；（b）为SF6/O2等离子体清洗，腔室压力为2.66 Pa；（c）为腔室压力为11.31 Pa；（d）为纯Cl2等离子体清洗，腔室压力为1.33 Pa、射频源功率为450 W.

Fig. 11 Chemical composition changes of the Al2O3 sample[42]

图12 Al2O3试样化学成分的变化[42]注：（a）为SF6/O2等离子体清洗；（b）（c）（d）分别为BCl3/Ar等离子体清洗10，20，40 s.

Fig. 12 Chemical composition changes of the Al2O3 sample[42]

图13 Al2O3试样的Al 2p XPS谱[42]注：（a）为清洗前的Al2O3试样；（b）（c）分别为SF6/O2等离子体清洗60，300 s；（d）SiCl4/Cl2等离子体清洗20 s.

Fig. 13 Al 2p XPS spectra of the Al2O3 sample [42]

图14 Al2O3 试样化学成分的变化[42].注：（a）为清洗前的Al2O3试样；（b）为SF6/O2等离子体清洗；（c）（d）分别为SiCl4/Cl2等离子体清洗15 s，120 s.

Fig. 14 Chemical composition changes of the Al2O3 sample[42]

图15 远程等离子体源清洗腔室的示意图[50]

Fig. 15 Schematic of using remote plasma source for chamber cleaning [50]

图16 等离子体清洗过程中铝合金样品的化学成分转变[51]（a）—Al（2p）；（b）—F（1s）；（c）—O（1s）；（d）—C（1s）.

Fig. 16 Chemical composition changes of the aluminum alloy sample during plasma cleaning[51]

图17 经历150 h NF3等离子体清洗后氧化铝视窗镜的截面形貌[45]（a）—原位清洗；（b）—远程微波清洗.

Fig. 17 Cross-sectional morphology of the Al2O3 window after 150 h cleaning by NF3 plasma[45]

图18 Non-Ce试样和3 mM Ce试样释放颗粒的差异[52]

Fig. 18 Variations in the generated particles between Non-Ce and 3 mM Ce samples[52]

图19 暴露于等离子体前后，阳极氧化涂层的击穿电压变化[53]

Fig. 19 Breakdown voltage changes of the anodized coating before and after plasma exposure[53]

图20 等离子体刻蚀过程中的颗粒原位监测[53]（a）—CF4/O2/Ar等离子体；（b）—NF3/O2/Ar等离子体.

Fig. 20 In-situ particle monitoring during plasma etching[53]

图21 阳极氧化涂层截面形貌[13,54]（a）—6061铝合金；（b）—纯铝.

Fig. 21 Cross-sectional morphology of the anodized coating[13,54]

图22 Y2O3试样化学成分的变化[15]注：（a）为清洗前的Y2O3试样；（b）为使用HBr/Cl2/O2等离子体刻蚀硅晶圆后；（c）为SF6/O2等离子体清洗80 s；（d）为SF6/O2等离子体清洗1 200 s.

Fig. 22 Chemical composition changes of the Y2O3 sample[15]

图23 Y2O3涂层表面剥落颗粒的TEM图像及元素分析[63].（a）—颗粒形貌；（b）—颗粒成分；（c）—颗粒形貌；（d）—高分辨图像.

Fig. 23 TEM images and elemental analysis of particles flaked from the Y2O3 coatings [63]

图24 不同沉积方法制备的Y2O3涂层的截面形貌[68]

Fig. 24 Cross-sectional morphology of the Y2O3 coatings prepared by various deposition methods[68]

图25 不同材料Cl原子的表面复合系数随温度的变化[72]（a）—阳极氧化铝；（b）—石英；（c）—多晶硅.

Fig. 25 Cl atomic surface recombination coefficient as a function of surface temperatures for various materials[72]

图26 不同表面状态的反应腔室的化学成分[74-75]注：（a～b）为SiO x Cl y 涂层腔室；（c～d）为AlF3涂层腔室.

Fig. 26 Chemical composition of the reactor walls at various surface conditions[74-75]

图27 硅的刻蚀轮廓[15]（a）—AlF3涂层腔室；（b）—SiO x Cl y 涂层腔室.

Fig. 27 Etching profile of the silicon gates[15]

图28 沉积的Si3N4，SiO2膜层厚度、均匀性随腔室使用次数的变化[14]（a）—Si3N4膜层厚度；（b）—SiO2膜层厚度；（c）—Si3N4膜层均匀性；（d）—SiO2膜层均匀性.

Fig. 28 Variation in Si3N4 and SiO2 thickness, thickness uniformity with number of chamber use[14]

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