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球磨时间对自钝化钨合金的组织结构和抗氧化性能的影响

陈时杰 叶超 柳炜 薛丽红 周启来 尹圣铭 严有为

陈时杰, 叶超, 柳炜, 等. 球磨时间对自钝化钨合金的组织结构和抗氧化性能的影响[J]. 复合材料学报, 2023, 40(8): 4531-4538. doi: 10.13801/j.cnki.fhclxb.20221115.001
引用本文: 陈时杰, 叶超, 柳炜, 等. 球磨时间对自钝化钨合金的组织结构和抗氧化性能的影响[J]. 复合材料学报, 2023, 40(8): 4531-4538. doi: 10.13801/j.cnki.fhclxb.20221115.001
CHEN Shijie, YE Chao, LIU Wei, et al. Effect of ball milling time on microstructure and oxidation resistance of self-passivating W alloys[J]. Acta Materiae Compositae Sinica, 2023, 40(8): 4531-4538. doi: 10.13801/j.cnki.fhclxb.20221115.001
Citation: CHEN Shijie, YE Chao, LIU Wei, et al. Effect of ball milling time on microstructure and oxidation resistance of self-passivating W alloys[J]. Acta Materiae Compositae Sinica, 2023, 40(8): 4531-4538. doi: 10.13801/j.cnki.fhclxb.20221115.001

球磨时间对自钝化钨合金的组织结构和抗氧化性能的影响

doi: 10.13801/j.cnki.fhclxb.20221115.001
基金项目: 国家磁约束核聚变能发展研究专项(2018 YFE0306104);材料成形与模具技术国家重点实验室开放课题研究基金(P2023-024)
详细信息
    通讯作者:

    薛丽红,博士,副教授,硕士生导师,研究方向为功能/结构复合材料 E-mail: xuelh@hust.edu.cn

  • 中图分类号: TB331

Effect of ball milling time on microstructure and oxidation resistance of self-passivating W alloys

Funds: National MCF Energy R&D Program (2018 YFE0306104); State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology (P2023-024)
  • 摘要: 自钝化W合金具有优异的抗高温氧化性能,可望用于高温环境中的关键部件。为了揭示合金的组织结构与高温抗氧化性能之间关系,采用机械合金化法结合放电等离子体烧结技术制备了自钝化W-Si合金,研究了不同机械合金化时间对合金显微组织结构的影响,并探究了合金的抗高温氧化性能。结果表明:合金由W、W5Si3和SiOx组成,当球磨时间由4 h增加到20 h,合金中SiOx的含量由16.2%增加到23.6%,而W5Si3的含量由57.8%降低到43.6%,且W和W5Si3的晶粒尺寸均减小,晶粒的细化有助于合金显微硬度的提高。在1000 ℃氧化10 h后,球磨4 h制得的合金增重为37.4 mg,而球磨20 h制得的合金增重达到了141.6 mg,它们的氧化层厚度分别约为167.0 μm和415.7 μm。球磨时间短制得的合金具有更优异的抗氧化性能,这是由于其W5Si3为连续相。W5Si3原位氧化形成的WO3/SiO2复合氧化物亦为连续相,形成了保护性氧化层,对合金的内氧化起到了有效的抑制作用。

     

  • 图  1  球磨不同时间的W-Si粉末的背散射SEM图像:(a) 4 h;(b) 20 h

    Figure  1.  Backscatter SEM images of W-Si powders ball milled for different time: (a) 4 h; (b) 20 h

    图  2  球磨4 h和20 h后的W-Si粉末的XRD图谱

    Figure  2.  XRD patterns of W-Si powders after ball milling for 4 h and 20 h

    图  3  球磨4 h和20 h的W-Si粉末制得的合金的XRD图谱

    Figure  3.  XRD patterns of the alloys made from the W-Si powders milled for 4 h and 20 h

    图  4  W-Si合金表面的背散射SEM图像 ((a1), (b1)) 和断口SEM图像 ((a2), (b2)):(a) 4 h;(b) 20 h

    A, B, C—Three different phases

    Figure  4.  Surface backscatter SEM images ((a1), (b1)) and fracture SEM images ((a2), (b2)) of the W-Si alloys: (a) 4 h;(b) 20 h

    图  5  球磨4 h和20 h的W-Si粉末制得的合金的氧化增重图

    Δm—Quality difference before and after oxidation

    Figure  5.  Oxidation mass gain of the alloys made from the W-Si powders milled for 4 h and 20 h

    图  6  W-Si合金分别氧化0 h、2 h和10 h的XRD图谱:(a) 球磨4 h;(b) 球磨20 h

    Figure  6.  XRD patterns of the W-Si alloys oxidized for 0 h, 2 h and 10 h, respectively: (a) Milled for 4 h; (b) Milled for 20 h

    图  7  W-Si合金在1000℃氧化不同时间的氧化层的SEM图像:((a1)~(a3)) 球磨4 h粉末制得的合金氧化0 h、2 h的合金表面和氧化2 h的氧化层侧表面;((b1)~(b3)) 球磨20 h粉末制得的合金氧化0 h、2 h的合金表面和氧化2 h的氧化层侧表面

    Figure  7.  SEM images of the oxide layer of the W-Si alloys oxidized for different time: ((a1)-(a3)) Alloy made from the powder milled for 4 h with surface oxidized for 0 h, 2 h and side surface oxidized for 2 h; ((b1)-(b3)) Alloy made from the powder milled for 20 h with surface oxidized for 0 h, 2 h and side surface oxidized for 2 h

    图  8  1000℃氧化2 h的W-Si合金截面的背散射SEM图像:(a) 球磨4 h粉末制得的合金;(b) 球磨20 h粉末制得的合金

    Figure  8.  Backscatter SEM images of the cross-sections of the W-Si alloys oxidized at 1000℃ for 2 h: (a) Milled for 4 h; (b) Milled for 20 h

    表  1  粉末中W的晶粒尺寸和Si在W中的固溶度

    Table  1.   Grain size of W and solid solubility of Si in W for the powders

    Ball milling time/hGrain size/nmSolid solubility/at%
    441.826.81
    2018.916.86
    下载: 导出CSV

    表  2  不同球磨时间制得的W-Si合金中各个相的面积含量

    Table  2.   Area content of each phases in the W-Si alloys prepared by different ball milling time

    W-Si alloySiOx/%W5Si3/%W/%
    Alloy made from the
    powder milled for 4 h
    16.257.826.0
    Alloy made from the
    powder milled for 20 h
    23.643.632.8
    下载: 导出CSV
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  • 收稿日期:  2022-09-15
  • 修回日期:  2022-11-07
  • 录用日期:  2022-11-10
  • 网络出版日期:  2022-11-17
  • 刊出日期:  2023-08-15

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