Szkudlarek Aleksandra, Rodrigues Vaz Alfredo, Zhang Yucheng, Rudkowski Andrzej, Kapusta Czesław, Erni Rolf, Moshkalev Stanislav, Utke Ivo
Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, 3602 Thun, Switzerland ; AGH University of Science and Technology, Academic Centre for Materials and Nanotechnology, al. A. Mickiewicza 30, 30-059 Krakow, Poland.
Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstrasse 39, 3602 Thun, Switzerland ; Center for Semiconductor Components, State University of Campinas, 13083-870, Campinas, SP, Brazil.
Beilstein J Nanotechnol. 2015 Jul 13;6:1508-17. doi: 10.3762/bjnano.6.156. eCollection 2015.
In this paper we study in detail the post-growth annealing of a copper-containing material deposited with focused electron beam induced deposition (FEBID). The organometallic precursor Cu(II)(hfac)2 was used for deposition and the results were compared to that of compared to earlier experiments with (hfac)Cu(I)(VTMS) and (hfac)Cu(I)(DMB). Transmission electron microscopy revealed the deposition of amorphous material from Cu(II)(hfac)2. In contrast, as-deposited material from (hfac)Cu(I)(VTMS) and (hfac)Cu(I)(DMB) was nano-composite with Cu nanocrystals dispersed in a carbonaceous matrix. After annealing at around 150-200 °C all deposits showed the formation of pure Cu nanocrystals at the outer surface of the initial deposit due to the migration of Cu atoms from the carbonaceous matrix containing the elements carbon, oxygen, and fluorine. Post-irradiation of deposits with 200 keV electrons in a transmission electron microscope favored the formation of Cu nanocrystals within the carbonaceous matrix of freestanding rods and suppressed the formation on their surface. Electrical four-point measurements on FEBID lines from Cu(hfac)2 showed five orders of magnitude improvement in conductivity when being annealed conventionally and by laser-induced heating in the scanning electron microscope chamber.
在本文中，我们详细研究了通过聚焦电子束诱导沉积（FEBID）制备的含铜材料的生长后退火。使用有机金属前驱体Cu(II)(hfac)2进行沉积，并将结果与早期使用(hfac)Cu(I)(VTMS)和(hfac)Cu(I)(DMB)的实验结果进行比较。透射电子显微镜显示了由Cu(II)(hfac)2沉积的非晶态材料。相比之下，由(hfac)Cu(I)(VTMS)和(hfac)Cu(I)(DMB)沉积的材料是纳米复合材料，其中Cu纳米晶体分散在碳质基质中。在150 - 200°C左右退火后，由于Cu原子从含有碳、氧和氟元素的碳质基质中迁移，所有沉积物在初始沉积物的外表面都显示出纯Cu纳米晶体的形成。在透射电子显微镜中用200 keV电子对沉积物进行辐照后，有利于在独立棒材的碳质基质中形成Cu纳米晶体，并抑制其表面的形成。对来自Cu(hfac)2的FEBID线进行的四点电学测量表明，在传统退火和扫描电子显微镜腔室中通过激光诱导加热时，电导率提高了五个数量级。
