Applied Microscopy

Korean Society of Microscopy (한국현미경학회)
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Structural and Morphological Changes of Co Nanoparticles and Au-10at.%Pd Thin Film Studied by in Situ Heating in a Transmission Electron Microscope

  • Ji, Yoon-Beom (Research & Development, Sung-Il Turbine Co., Ltd.) ;
  • Park, Hyun Soon (Department of Materials Science and Engineering, Inha University)
  • Received : 2017.08.22
  • Accepted : 2017.09.06
  • Published : 2017.09.30
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Abstract

The microstructural changes in Co nanoparticles and an Au-10at.%Pd thin film have been investigated using an in situ heating holder with a micro-electro-mechanical system (MEMS). In Co nanoparticles, two phases (face-centered cubic and hexagonal close-packed crystal structures) were found to coexist at room temperature and microstructures at temperatures, higher than $1,000^{\circ}C$, were observed with a quick response time and significant stability. The actual temperature of each specimen was directly estimated from the changes in the lattice spacing (Bragg-peak separation). For the Au-10at.%Pd thin film, at a set temperature of $680^{\circ}C$, the actual temperature of the sample was estimated to be $1,020^{\circ}C{\pm}123^{\circ}C$. Note that the specimen temperature should be carefully evaluated because of the undesired effects, i.e., the temperature non-uniformity due to the sample design of the MEMS chip, and distortion due to thermal expansion.

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References

  1. Allard L F, Bigelow W C, Jose-Yacaman M, Nackashi D P, Damiano J, and Mick S E (2009) A new MEMS-based system for ultra-high-resolution imaging at elevated temperature. Microscopy Research and Technique 72, 208-215. https://doi.org/10.1002/jemt.20673
  2. Asoro M A, Kovar D, and Ferreira P J (2013) In-situ transmission electron microscopy observation of sublimation in silver nanoparticles. J. ACS Nano. 7, 7844-7852. https://doi.org/10.1021/nn402771j
  3. Bao Y, Beermanm M, Pakhomov A B, and Krishnan K M (2005) Controlled crystalline structure and surface stability of cobalt nanocrystals. J. Phys. Chem. B 109, 7220-7222. https://doi.org/10.1021/jp044363n
  4. Barwick B, Park H S, Kwon O H, Baskin J S, and Zewail A H (2008) 4D imaging of transient structures and morphologies in ultrafast electron microscopy. Science 322, 1227-1231. https://doi.org/10.1126/science.1164000
  5. Gontard L C, Dunin-Borkowski R E, Fernandez F, Ozkaya D, and Kasama T (2014) Tomographic heating holder for in situ TEM: Study of Pt/C and PtPd/Al2O3 catalysts as a function of temperature. Microsc. Microanal. 20, 982-990.
  6. Ivanov V, Kotov Y A, and Samatov O H (1995) Synthesis and dynamic compaction of ceramic nano powders by techniques based on electric pulsed power. Nanostructured Materials 6, 287-290. https://doi.org/10.1016/0965-9773(95)00054-2
  7. Kim T H, Bae J H, Lee J W, Shin K, Lee J H, Kim M Y, and Yang C W (2015) Temperature calibration of a specimen-heating holder for transmission electron microscopy. Appl. Microsc. 2, 95-100.
  8. Lee G H, Park J H, Rhee C K, and Kim W W (2003) Fabrication of Al nano powders by pulsed wire evaporation (PWE) method. J. Ind. Eng. Chem. 9, 71-75.
  9. Matveev V V, Baranov D A, Yurkov G Y, Akatiev N G, Dotsenko I P, and Gubin S P (2006) Cobalt nanoparticles with preferential hcp structure: a confirmation by X-ray diffraction and NMR. Chemical Physics Letters 422, 402-405. https://doi.org/10.1016/j.cplett.2006.02.099
  10. Okamoto H and Massalski T B (1985) The Au-Pd (Gold-Palladium) system. Bulletin of Alloy Phase Diagrams 6, 229-235. https://doi.org/10.1007/BF02880404
  11. Park H S, Baskin J S, Barwick B, Kwon O H, and Zewail A H (2009) 4D ultrafast electron microscopy: imaging of atomic motions, acoustic resonances, and moire fringe dynamics. Ultramicroscopy 110, 7-19. https://doi.org/10.1016/j.ultramic.2009.08.005
  12. Saka H, Kamino T, Arai S, and Sasaki K (2008) In situ heating transmission elecctron microscopy. J. MRS Bulletin 33, 93-100. https://doi.org/10.1557/mrs2008.21
  13. Seo W S, Shim J H, Oh S J, Lee E K, Hur N H, and Park J T (2005) Phase-and size-controlled synthesis of hexagonal and cubic CoO nanocrystals. J. Am. Chrm. Soc. 127, 6188-6189. https://doi.org/10.1021/ja050359t
  14. Takeo K, Toshie Y, Mitsuru K, Akira W, and Yasuhira N (2006) Development of a specimen heating holder with an evaporator and gas injector and its application for catalyst. Journal of Electron Microscopy 55, 245-252. https://doi.org/10.1093/jmicro/dfl032
  15. Yoo C, Soderlind P, and Cynn H (1998) The phase diagram of cobalt at high pressure and temperature: the stability of ${\gamma}$(fcc)-cobalt and new ${\varepsilon}$'(dhcp)-cobalt. J. Phys.: Condens. Matter. 10, 311-318. https://doi.org/10.1088/0953-8984/10/20/001
  16. Zhang Z and Su D (2009) Behavior of TEM metal grids during in-situ heating experiment. Ultramicroscopy 109, 766-774. https://doi.org/10.1016/j.ultramic.2009.01.015