表面纳米化材料横截面透射电镜试样的制备
Preparation for Cross-sectional TEM Specimen Treated by Self Surface Nanocrystallization
摘 要
通过严重塑性变形法得到的表面纳米化材料,由于近表层有较高的残余应力,其横截面透射电镜试样的制备比一般的电镜试样困难。介绍了一种机械预减薄后,用Teflon板夹持试样与铜环进行树脂的热固化,再直接用离子减薄的制样方法。对表面纳米化后TC4钛合金的横截面试样制备结果表明,该方法避免了试样弯曲变形,可以得到适合于透射电镜观察的横截面试样。
透射电镜
试样制备
横截面
surface nanocrystallization
TEM
specimen preparation
cross section
Abstract
On account of the high residual stress in the near surface layer of the surface-nanocrystallized material by severe plastic deformation,it is rather difficult to prepare the cross-sectional specimens for transmission electron microscopy (TEM) observation. A new specimen preparation method was presented that the specimen was ion milled directly after mechanical pre-thinning. The pre-thinned specimen was glued on a copper ring with Gatan G2 epoxy resin and was cured before ion milling. The points were that the pre-thinning procedure was performed by plane grinding and the specimen and the copper ring was retained by two Teflon plates when the resin was being cured. Therefore,the easy-happened bend of the specimen due to the residual stress was eliminated. The experimental results of TC4 titanium alloy specimens preparation treated by self surface nanocrystallization showed that the specimens had no bending deformation and had large cross-sectional thin area. The subsequent TEM observation of the specimens was achieved successfully.
中图分类号 TG146.2 TN16
所属栏目 试验技术与方法
基金项目
收稿日期 2009/3/3
修改稿日期
网络出版日期
作者单位点击查看
备注陈春焕(1970-),男,副教授。
引用该论文: CHEN Chun-huan,REN Rui-ming,SONG Ming-hui,KAZUO Furuya. Preparation for Cross-sectional TEM Specimen Treated by Self Surface Nanocrystallization[J]. Physical Testing and Chemical Analysis part A:Physical Testing, 2009, 45(11): 680～683
陈春焕,任瑞铭,宋明晖,古屋一夫. 表面纳米化材料横截面透射电镜试样的制备[J]. 理化检验－物理分册, 2009, 45(11): 680～683
被引情况:
【1】王燕飞,黄宛真,郑遗凡,胡仙超,苏伟涛,杨倩, "脆性材料截面透射电镜样品的制备",理化检验－物理分册 47, 225-228(2011)
【2】杨倩,黄宛真,郑遗凡,胡仙超,王燕飞, "一种制备透射电镜截面样品的新方法",理化检验－物理分册 48, 91-94(2012)
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【4】徐滨士. 纳米表面工程[M]. 北京：化学工业出版社,2003．
【5】ZHU K Y,VASSEL A,BRISSET F,et al. Nanostructure formation mechanism of α-titanium using SMAT[J]. Acta Materialia,2004,52(14): 4101-4110．
【6】UMEMOTO M,TODAKA K,TSUCHIYA K. Formation of nanocrystalline structure in carbon steels by ball drop and particle impact techniques[J]. Materials Science and Engineering A,2004,375-377(15): 899-904．
【7】雍兴平,刘刚,吕坚,等. 低碳钢表面纳米化处理及结构特征[J]. 金属学报,2002,38(2): 157-160．
【8】温爱玲,陈春焕,郑德有,等. 高能喷丸表面纳米化对工业纯钛组织性能的影响[J]. 表面技术,2003,32(3): 16-18．
【9】张淑兰,陈怀宁,林泉洪,等. 工业纯钛的表面纳米化及其机制[J]. 有色金属,2003,55(4): 5-8．
【10】ZHANG H W,HEI Z K,LIU G,et al. Formation of nanostructured surface layer on AISI 304 stainless steel by means of surface mechanical attrition treatment[J]. Acta Materialia,2003,51(7): 1871-1881．
【11】WANG K,TAO N R,LIU G,et al. Plastic strain-induced grain refinement at the nanometer scale in copper[J]. Acta Materialia,2006,54(19): 5281．
【12】戎咏华. 分析电子显微学导论[M]. 北京：高等教育出版社,2006．
【13】ZHANG XIAO-FENG,ZHANG ZE. Progress in Transmission Electron Microscopy 1[M]. Beijing: Tsinghua University Press,1999．
【14】WANGNER L. Mechanical surface treatments on titanium,aluminum and magnesium alloys[J]. Materials Science and Engineering A,1999,263(2): 210．
【15】COSTA M Y P,VOORWALD H J C,PIGATIN W L,et al. Evaluation of shot peening on the fatigue strength of anodized Ti-6Al-4V alloy[J]. Materials Research,2006,9(1): 107-109．
【16】张洪旺,刘刚,黑祖昆,等. 表面机械研磨诱导AISI 304不锈钢表层纳米化——Ⅱ.晶粒细化机理[J]. 金属学报,2003,39(4): 347-350．
【17】TAO N R,WANG Z B,TONG W P,et al. An investigation of surface nanocrystallization mechanism in Fe induced by surface mechanical attrition treatment[J]. Acta Materialia,2002,50(18): 4603-4616．
【18】WU X,TAO N,HONG Y,et al. Microstructure and evolution of mechanically-induced ultrafine grain in surface layer of Al-alloy subjected to USSP[J]. Acta Materialia,2002,50(8): 2075-2084 ．
【19】郑艳霞. 工业纯钛室温ECAP与冷轧变形及组织性能研究[D]. 西安：西安建筑科技大学,2007．
【20】ZHANG YU-JUN,CHEN CHUN-HUAN,REN RUI-MING. Thermal stability of surface layer microstructures of commercially pure titanium treated by high energy shot peening[J]. Materials Protection,2004,37(9): 238-240．
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