基于FIB加工和SEM-EDS技术联用对共格BCC/B2高熵合金的元素分布表征分析
史淑艳,王成林,戚 琳,马 跃,邹龙江
(大连理工大学材料科学与工程学院,辽宁 大连 116024 )
摘 要 BCC/B2高熵合金中体心立方结构(body centered cube, BCC)纳米粒子影响其软磁性能和高温力学性能。然而,扫描电子显微镜-能量色散谱仪(scanning electron microscopy - X-ray energy dispersive spectroscopy, SEM-EDS)难以表征BCC纳米粒子的元素分布。本文利用聚焦离子束(focused ion beam,FIB)和SEM-EDS联用,制备BCC/B2高熵合金的纳米尺度薄片,并对其元素分布进行了研究。结果表明,Al17.65Co47.06Fe23.53Cr11.76高熵合金微观组织是由B2相与共格的BCC相构成,其中BCC粒子约为20~40 nm。对比SEM-EDS对块体试样和FIB制备的纳米尺度的薄片元素分布结果,FIB制备的纳米薄片提高了EDS的分辨率,BCC纳米粒子富集Cr元素,且B2基体相富集Al、Co和Fe元素。电子的加速电压和束流强度影响纳米薄片中BCC纳米粒子元素分布表征结果的准确性,其中30 kV 6.4 nA下元素分布表征结果的准确度最高。
关键词 高熵合金;纳米颗粒;元素分布;聚焦离子束;扫描电子显微镜-能量色散谱仪
中图分类号:TB331;TG113;TG115. 21 文献标识码:Adoi:10.3969/j.issn.1000-6281.2022.03.006
Elemental distribution of BCC nanoparticles in coherent BCC/B2 high entropy alloy by focused ion beam processing and scanning electron microscopy
SHI Shu-yan, WANG Cheng-lin, QI Lin, MA Yue, ZOU Long-jiang
(School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China)
Abstract In BCC/B2 high entropy alloy, body centered cube (BCC) nanoparticles affect the soft magnetic properties and high temperature mechanical properties. However, the elemental distribution of BCC nanoparticles is difficult to be characterized by scanning electron microscope-energy dispersion spectroscopy (SEM-EDS). In this paper, focused ion beam (FIB) and SEM-EDS were used to prepare nanoscale sheet of BCC/B2 high entropy alloy, and the elemental distribution of the nanoscale sheet was studied. The microstructure of Al17.65Co47.06Fe23.53Cr11.76 high entropy alloy is coherent with BCC/B2 phases, and the size distribution of BCC particles is 20-40 nm. When SEM-EDS was used to analyze the elemental distribution of the block sample and the nanoscale sheet sample prepared by FIB, the nanosheet prepared by FIB improves the resolution of EDS, BCC nanoparticles are enriched in Cr, and B2 matrix is enriched in Al, Co and Fe. The accelerating voltage and beam intensity affect the accuracy of the element distribution results of BCC nanoparticles in the nanosheets, and the highest accuracy of the element distribution results is obtained at 30 kV 6.4 nA.
Keywords high entropy alloy; nano-particles; elemental distribution; focused ion beam; scanning electron microscope-energy dispersion spectrometer
“全文下载请到同方知网,万方数据库或重庆维普等数据库中下载!”
[1] 韩劲,倪志铭,杨根林,等. 高温高强度Fe-Co软磁合金研制[J]. 功能材料,2015,21:21076-21080.
[2] VARGA L K. Soft magnetic nanocomposites for high-frequency and high-temperature applications [J]. Journal of Magnetism and Magnetic Materials,2007,316(2):442-447.
[3] FINGERS R T,RUBERTUS C S. Application of high temperature magnetic materials [J]. IEEE Transactions on Magnetics, 2000,36(5):3373-3375.
[4] YOSHIZAWA Y,OGUMA S,YAMAUCHI K. New Fe‐based soft magnetic alloys composed of ultrafine grain structure [J]. Journal of Applied Physics, 1988,64(10):6044-6046.
[5] DING Q Q,LI S X,HEN L Q,et al. Re segregation at interfacial dislocation network in a nickel-based superalloy [J]. Acta Materialia,2018,154:137-146.
[6] CANTOR B,CHANG I T H,KNIGHT P,et al. Microstructural development in equiatomic multicomponent alloys [J]. Materials Science and Engineering: A,2004,375-377:213-218.
[7] YEH J W,CHEN S K,LIN S J,et al. Nanostructured high-entropy alloys with multiple principal elements: novel alloy design concepts and outcomes [J]. Advanced Engineering Materials,2004,6(5):299-303.
[8] ZHANG Y,ZUO T T,TANG Z,et al. Microstructures and properties of high-entropy alloys [J]. Progress in Materials Science, 2014,61(8):1-93.
[9] 栾亨伟,赵威,姚可夫. 高熵合金的力学性能及功能性能研究进展[J]. 材料热处理学报,2020,41(1):1-11.
[10] LI Z,BAI G,LIU X,et al. Tuning phase constitution and magnetic properties by composition in FeCoNiAlMn high-entropy alloys [J]. Journal of Alloys and Compounds, 2020,845:156204.
[11] LIU C,PENG W,JIANG C S,et al. Composition and phase structure dependence of mechanical and magnetic properties for AlCoCuFeNix high entropy alloys [J]. Journal of Materials Science and Technology,2019,035:1175-1183.
[12] KOZELJ P,VRTNIK S,JELEN A,et al. Discovery of a FeCoNiPdCu high‐entropy alloy with excellent magnetic softness [J]. Advanced Engineering Materials,2018,21(5):1801055.
[13] ZHANG H,YANG Y X,LIU L,et al. A novel FeCoNiCr0.2Si0.2 high entropy alloy with an excellent balance of mechanical and soft magnetic properties [J]. Journal of Magnetism and Magnetic Materials,2019,478:116-121.
[14] CHEN C,ZHANG H,FAN Y Z,et al. A novel ultrafine-grained high entropy alloy with excellent combination of mechanical and soft magnetic properties [J]. Journal of Magnetism and Magnetic Materials,2020,502:166513.
[15] MA Y,WANG Q,ZHOU X,et al. A novel soft-magnetic B2-based multiprincipal-element alloy with a uniform distribution of coherent body-centered-cubic nanoprecipitates [J]. Advanced Materials,2021,33:2006723.
[16] 黎爽,邓平晔,蔡锴,等. 一种提高扫描电子显微镜-能谱空间分辨率的方法[J]. 电子显微学报,2015,34(3):240-249.
[17] 黎爽,邓平晔. 提高热场扫描电镜能谱空间分辨率的方法研究[J]. 分析科学学报,2018,34(6):824-828.
[18] 任小明,蔡志伟. 提高扫描电镜能谱空间分辨率的方法研究[J]. 分析科学学报,2020,36(4):579-583.
[19] 瞿敏妮,沈贇靓,乌李瑛,等. 聚焦离子束对铌酸锂表面加工的形貌控制研究[J].电子显微学报,2020,39(2):189-195.
[20] 周玲玲,孙威. FIB加工、扫描及透射电子显微镜相结合的复杂合金相层状组织表征[J]. 电子显微学报,2018,37(6):590-595.