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In Situ Thermal Annealing Transmission Electron Microscopy (TEM) Investigation of III/V Semiconductor Heterostructures Using a Setup for Safe Usage of Toxic and Pyrophoric Gases

Published online by Cambridge University Press:  08 August 2017

Rainer Straubinger
Affiliation:
Faculty of Physics and Materials Science Center, Philipps-Universitat Marburg Ringgold, Hans-Meerwein-Straße 6, Marburg, Hessen 35032, Germany
Andreas Beyer*
Affiliation:
Faculty of Physics and Materials Science Center, Philipps-Universitat Marburg Ringgold, Hans-Meerwein-Straße 6, Marburg, Hessen 35032, Germany
Thomas Ochs
Affiliation:
Faculty of Physics and Materials Science Center, Philipps-Universitat Marburg Ringgold, Hans-Meerwein-Straße 6, Marburg, Hessen 35032, Germany
Wolfgang Stolz
Affiliation:
Faculty of Physics and Materials Science Center, Philipps-Universitat Marburg Ringgold, Hans-Meerwein-Straße 6, Marburg, Hessen 35032, Germany
Kerstin Volz
Affiliation:
Faculty of Physics and Materials Science Center, Philipps-Universitat Marburg Ringgold, Hans-Meerwein-Straße 6, Marburg, Hessen 35032, Germany
*
*Corresponding author. [email protected]
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Abstract

In this study we compare two thermal annealing series of III/V semiconductor heterostructures on Si, where during the first series nitrogen is present in the in situ holder. The second, comparative, measurement is done in a tertiarybutylphosphine (TBP) environment. The sample annealed in a TBP environment shows favorable thermal stability up to 500°C compared to the unstabilized sample, which begins to degrade at less than 300°C. Evaporation of P from the material is tracked qualitatively by measuring the thickness of the sample during thermal annealing with and without stabilization. Finally, we investigate the in situ thermal annealing processes at atomic resolution. Here it is possible to study phase separation as well as the diffusion of As from a Ga(NAsP) quantum well in the surrounding GaP material during thermal annealing. To make these investigations possible we developed an extension for our in situ transmission electron microscopy setup for the safe usage of toxic and pyrophoric III/V semiconductor precursors. A commercially available gas cell and gas supply system were expanded with a gas mixing system, an appropriate toxic gas monitoring system and a gas scrubbing system. These components allow in situ studies of semiconductor growth and annealing under the purity conditions required for these materials.

Type
Materials Science Applications
Copyright
© Microscopy Society of America 2017 

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References

Allard, L.F., Overbury, S.H., Bigelow, W.C., Katz, M.B., Nackashi, D.P. & Damiano, J. (2012). Novel MEMS-based gas-cell/heating specimen holder provides advanced imaging capabilities for in situ reaction studies. Microsc Microanal 18, 656666.CrossRefGoogle ScholarPubMed
Beyer, A., Belz, J., Knaub, N., Jandieri, K. & Volz, K. (2016). Influence of spatial and temporal coherences on atomic resolution high angle annular dark field imaging. Ultramicroscopy 169, 110.CrossRefGoogle ScholarPubMed
Buyanova, I.A, Pozina, G., Hai, P.N., Thinh, N.Q., Bergman, J.P., Chen, W.M., Xin, H.P. & Tu, C.W. (2000). Mechanism for rapid thermal annealing improvements in undoped GaNxAs1−x / GaAs structures grown by molecular beam epitaxy. Appl Phys Lett 77, 2325.CrossRefGoogle Scholar
Diaz, R.E., Sharma, R., Jarvis, K., Zhang, Q. & Mahajan, S. (2012). Direct observation of nucleation and early stages of growth of GaN nanowires. J Cryst Growth 341, 16.CrossRefGoogle Scholar
Gies, S., Zimprich, M., Wegele, T., Kruska, C., Beyer, A., Stolz, W., Volz, K. & Heimbrodt, W. (2014). Annealing effects on the composition and disorder of Ga(N,As,P) quantum wells on silicon substrates for laser application. J Cryst Growth 402, 169174.CrossRefGoogle Scholar
He, D.S. & Li, Z.Y. (2014). A practical approach to quantify the ADF detector in STEM. J Phys Conf Ser 522, 12017.CrossRefGoogle Scholar
Kobayashi, N. & Kobayashi, Y. (1991). As and P deposition from III-V semiconductor surface in metalorganic chemical vapor deposition studied by suface photo-absorption. Jpn J Appl Phys 30, 16991701.CrossRefGoogle Scholar
Kunert, B., Reinhard, S., Koch, J., Lampalzer, M., Volz, K. & Stolz, W. (2006). First demonstration of electrical injection lasing in the novel dilute nitride Ga (NAsP)/GaP-material system. Physica Status Solidi (c) 3, 614618.CrossRefGoogle Scholar
Liebich, S., Zimprich, M., Beyer, A., Lange, C., Franzbach, D.J., Chatterjee, S., Hossain, N., Sweeney, S.J., Volz, K., Kunert, B. & Stolz, W. (2011). Laser operation of Ga(NAsP) lattice matched to (001) silicon substrate. Appl Phys Lett 99, 71109.CrossRefGoogle Scholar
Protochips (2016). Protochips http://www.protochips.com/.Google Scholar
Rosenauer, A. & Schowalter, M. (2007). STEMSIM—A new software tool for simulation of STEM HAADF Z-contrast imaging. In Microscopy of Semiconducting Materials (Proceedings in Physics), Cullis, A.G. & Midgley, P.A. (Eds.), pp. 169–172. Dordrecht, The Netherlands: Springer.Google Scholar
Schaffer, M., Schaffer, B. & Ramasse, Q. (2012). Sample preparation for atomic-resolution STEM at low voltages by FIB. Ultramicroscopy 114, 6271.CrossRefGoogle ScholarPubMed
Schowalter, M., Rosenauer, A., Titantah, J.T. & Lamoen, D. (2008). Computation and parametrization of the temperature dependence of Debye-Waller factors for group IV, III-V and II-VI semiconductors. Acta Crystallogr A Found Crystallogr 65, 517.CrossRefGoogle Scholar
Straubinger, R., Beyer, A. & Volz, K. (2016). Preparation and loading process of single crystalline samples into a gas environmental cell holder for in situ atomic resolution scanning transmission electron microscopic observation. Microsc Microanal 22, 515519.CrossRefGoogle ScholarPubMed
Volz, K., Beyer, A., Witte, W., Ohlmann, J., Nmeth, I., Kunert, B. & Stolz, W. (2011). GaP-nucleation on exact Si (0 0 1) substrates for III/V device integration. J Cryst Growth 315, 3747.CrossRefGoogle Scholar
Wegele, T., Beyer, A., Gies, S., Zimprich, M., Heimbrodt, W., Stolz, W. & Volz, K. (2016a). Correlation of the nanostructure with optoelectronic properties during rapid thermal annealing of Ga(NAsP) quantum wells grown on Si(001) substrates. J Appl Phys 119, 025705.CrossRefGoogle Scholar
Wegele, T., Beyer, A., Ludewig, P., Rosenow, P., Duschek, L., Jandieri, K., Tonner, R., Stolz, W. & Volz, K. (2016b). Interface morphology and composition of Ga(NAsP) quantum well structures for monolithically integrated LASERs on silicon substrates. J Phys D Appl Phys 49, 75108.CrossRefGoogle Scholar
Wen, C.Y., Tersoff, J., Hillerich, K., Reuter, M.C., Park, J.H., Kodambaka, S., Stach, E.A. & Ross, F.M. (2011). Periodically changing morphology of the growth interface in Si, Ge, and GaP nanowires. Phys Rev Lett 107, 14.CrossRefGoogle Scholar