Song Se Ahn, Zhang Wei, Sik Jeong Hong, Kim Jin-Gyu, Kim Youn-Joong
AE Center, Samsung Advanced Institute of Technology, Yongin, 446-712, Republic of Korea.
Ultramicroscopy. 2008 Oct;108(11):1408-19. doi: 10.1016/j.ultramic.2008.05.012. Epub 2008 Jun 19.
The phase transition phenomena of Ge2Sb2Te5 chalcogenides were investigated by in situ dynamic high-resolution transmission electron microscopy (HR-TEM) and electron energy loss spectroscopy (EELS). A 300kV field emission TEM and a 1250kV high voltage TEM were employed for the in situ heating experiments from 20 to 500 degrees C for undoped and 3wt% nitrogen-doped Ge2Sb2Te5 thin films deposited by DC sputtering. Crystallization of amorphous Ge2Sb2Te5 to its cubic structure phase started at 130 degrees C and then rapid crystal growth developed from cubic to hexagonal phase in the range of 130-350 degrees C; finally, the hexagonal crystals started to melt at 500 degrees C. For nitrogen-doped Ge2Sb2Te5, its crystallization from amorphous film occurred at higher temperature of ca. 200 degrees C, and the cubic and hexagonal phases were usually formed simultaneously without significant growth of crystals at further heating to 400 degrees C. EELS measurements showed that the electronic structures of Ge, Sb and Te stayed almost the same regardless of the amorphous, FCC and hexagonal phases. The nitrogen doped in Ge2Sb2Te5 was confirmed to exist as a nitride. Also, the doped nitrogen distributed homogeneously in both amorphous and crystalline phases. Localization of doped nitrogen was not found in the grain boundary of crystallized phases. The dynamic process of phase transition was enhanced by high-energy electron irradiation. Peeling of atomic layers in nitrogen-doped Ge2Sb2Te5 film was detected during heating assisted with electron beam irradiation.
通过原位动态高分辨率透射电子显微镜(HR-TEM)和电子能量损失谱(EELS)研究了Ge2Sb2Te5硫族化物的相变现象。采用300kV场发射TEM和1250kV高压TEM对通过直流溅射沉积的未掺杂和3wt%氮掺杂的Ge2Sb2Te5薄膜进行20至500摄氏度的原位加热实验。非晶态Ge2Sb2Te5向其立方结构相的结晶在130摄氏度开始,然后在130-350摄氏度范围内从立方相快速生长为六方相;最后,六方晶体在500摄氏度开始熔化。对于氮掺杂的Ge2Sb2Te5,其从非晶膜的结晶发生在约200摄氏度的较高温度下,并且在进一步加热到400摄氏度时,立方相和六方相通常同时形成,没有明显的晶体生长。EELS测量表明,无论处于非晶相、面心立方相和六方相,Ge、Sb和Te的电子结构几乎保持不变。证实掺杂在Ge2Sb2Te5中的氮以氮化物形式存在。而且,掺杂的氮在非晶相和结晶相中均均匀分布。在结晶相的晶界中未发现掺杂氮的局域化。高能电子辐照增强了相变的动态过程。在电子束辐照辅助加热过程中,检测到氮掺杂的Ge2Sb2Te5薄膜中原子层的剥离。