14Cr-ODS合金粉球磨过程中的显微结构变化及合金化进程
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摘要
利用OM、SEM、EDS和XRD等测试手段研究了球磨转速和球磨时间对14Cr-ODS合金粉的形貌、显微结构及物相的影响。结果表明,转速为250 r/min时,随着球磨时间的延长,粉末粒径增大,16 h时基本稳定;点阵参数增大,晶粒尺寸不断减小并趋于稳定;12 h时颗粒内部出现层状结构并不断细化直至消失,颗粒成分更接近名义成分。12 h时合金化已开始,持续球磨使合金化程度提高,30 h时基本实现合金化。合金化过程可分为包覆、粘结、分层、细化、均匀化5个阶段。当转速提高到300 r/min时,合金化进程加快。
The variation of morphology,microstructure and phase constituent of 14Cr-ODS( Oxide dispersion strengthened steel,ODS)powders during mechanical ball-milling were investigated by using optical microscopy( OM),scanning electron microscopy( SEM),energy dispersive X-ray spectroscopy( EDS) and X-ray diffraction( XRD). It is demonstrated that for a given rotating rate of 250 r / min,the size of powder particle increases gradually with increasing milling-time until 16 h. Moreover,their grain size is reduced down to a constant value and the lattice parameter becomes larger. For the powder sample mechanically milled for 12 h,the composition of particles is determined to be very close to the nominal one while the laminated structure can be observed,which however becomes invisible ultimately for the particle refinement. It is thus believed that the mechanical alloying starts to take place in the alloy system at about 12 h but is completed after 30 h. Consequently,the mechanical alloying process can be divided into five consecutive stages: cladding,bonding,laminating,refining and homogenization. Furthermore,it is found that the kinetics of mechanically alloying is speeded up with increasing the ball-milling speed.
The variation of morphology,microstructure and phase constituent of 14Cr-ODS( Oxide dispersion strengthened steel,ODS)powders during mechanical ball-milling were investigated by using optical microscopy( OM),scanning electron microscopy( SEM),energy dispersive X-ray spectroscopy( EDS) and X-ray diffraction( XRD). It is demonstrated that for a given rotating rate of 250 r / min,the size of powder particle increases gradually with increasing milling-time until 16 h. Moreover,their grain size is reduced down to a constant value and the lattice parameter becomes larger. For the powder sample mechanically milled for 12 h,the composition of particles is determined to be very close to the nominal one while the laminated structure can be observed,which however becomes invisible ultimately for the particle refinement. It is thus believed that the mechanical alloying starts to take place in the alloy system at about 12 h but is completed after 30 h. Consequently,the mechanical alloying process can be divided into five consecutive stages: cladding,bonding,laminating,refining and homogenization. Furthermore,it is found that the kinetics of mechanically alloying is speeded up with increasing the ball-milling speed.
引文
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[2]Hoelzer D T,Bentley J,Sokolov M A,et al.Influence of particle dispersions on the high-temperature strength of ferritic alloys[J].Journal of Nuclear Materials,2007,367/370(Part A):166-172.
[3]Oksiuta Z.High-temperature oxidation resistance of ultrafine-grained 14%Cr ODS ferritic steel[J].Journal of Materials Science,2013,48(13):4801-4805.
[4]Pareige P,Miller M K,Stoller R E,et al.Stability of nanometer-sized oxide clusters in mechanically-alloyed steel under ion-induced displacement cascade damage conditions[J].Journal of Nuclear Materials,2007,360(2):136-142.
[5]吕铮.聚变堆第一壁用纳米结构ODS钢的发展与前瞻[J].原子能科学技术,2011,45(9):1105-1111.LZheng.Development and prospect of nano-structured ODS steels for fusion reactor first wall application[J].Atomic Energy Science and Technology,2011,45(9):1105-1111.
[6]Yao Z H,Xiong W H,Yuan M,et al.Effects of mechanical alloying on characteristics of nanocrystalline Fe-Cr-W-Ti-Y2O3powders[J].Journal of Nuclear Materials,2010,403(1/3):198-203.
[7]Hoffmann J,Klimenkov M,Lindau R,et al.TEM study of mechanically alloyed ODS steel powder[J].Journal of Nuclear Materials,2012,428(1/3):165-169.
[8]Rahmanifard R,Farhangi H,Novinrooz A J.Optimization of mechanical alloying parameters in 12YWT ferritic steel nanocomposite[J].Materials Science and Engineering A,2010,527(26):6853-6857.
[9]Dousti B,Mojaver R,Shahverdi H R,et al.Microstructural evolution and chemical redistribution in Fe-Cr-W-Ti-Y2O3nanostructured powders prepared by ball milling[J].Journal of Alloys and Compounds,2013,577:409-416.
[10]何培,周张健,李明,等.机械合金化对ODS铁素体钢粉末的微观形貌和结构的影响[J].北京科技大学学报,2009,31(7):836-841.HE Pei,ZHOU Zhang-jian,LI Ming,et al.Effect of mechanical alloying on the microstructural properties of powder particles for oxide dispersion strengthened ferritic steels[J].Journal of University of Science and Technology Beijing,2009,31(7):836-841.
[11]何培,周张健,李明,等.初始原料和球磨气氛对ODS铁素体钢机械合金化的影响[J].材料工程,2010(9):20-24.HE Pei,ZHOU Zhang-jian,LI Ming,et al.Effect of starting materials and milling atmosphere on mechanical alloying of ODS ferritic steels[J].Journal of Materials Engineering,2010(9):20-24.