AVS 61st International Symposium & Exhibition
    Materials Characterization in the Semiconductor Industry Focus Topic Monday Sessions
       Session MC+2D+AP+AS-MoA

Paper MC+2D+AP+AS-MoA3
Determination of Growth Conditions for Highly Mismatched Alloys, Using In Situ Auger Electron Spectroscopy and Flux grading

Monday, November 10, 2014, 2:40 pm, Room 313

Session: Characterization of III-Vs (2:00-3:20 pm)/Photovoltaics, EUV masks, etc. (3:40-4:40 pm)
Presenter: Stefan Svensson, US Army Research Laboratory
Authors: S.P. Svensson, US Army Research Laboratory
W.L. Sarney, US Army Research Laboratory
M. Ting, Lawrence Berkeley National Laboratory
K.M. Yu, Lawrence Berkeley National Laboratory
L.W. Calley, Staib Instruments, Inc.
Correspondent: Click to Email

The electronic band structures of GaN can be effectively modified by the incorporation of Sb. Because of the high electronegativity mismatch between Sb and N growth of GaNSb by molecular beam epitaxy (MBE) must be done at relatively low temperatures and under N-rich condition in order to control the bandgap of the material. The Sb-flux must also be chosen carefully in relation to the growth rate and N-overpressure to control composition and crystallinity. These growth conditions represent a vast parameter space, which is extremely time-consuming to explore in a systematic fashion.

The typical approach for attacking such a problem is to judiciously select a limited set of parameter combinations based on experience and literature data. However, if growth windows are narrow there is no guarantee for success. To more quickly cover a larger parameter range we have grown a very limited number of samples but continuously varied one parameter at a time while employing a combination of in situ and ex situ probes that can reveal critical parameter points. The most novel piece of equipment is the in situ STAIB Auger Probe, which allows uninterrupted chemical analysis during crystal growth. In all of the following experiments the substrate temperature was fixed at 325 °C.

In one experiment we determined the transition between Ga- and N-rich MBE growth conditions of GaN by setting a fixed N-flow that generated a steady-state background chamber pressure of 1.5x10-5 Torr, while the Ga-source was set up to generate a linear flux ramp from 9.8x1016 to 3.9x1018 at/m2/s over two hours. During this ramp, the Auger electron signals for N (375 eV), and Ga (1050 eV) were continuously monitored. As expected, both the Ga and N signals increased as a GaN film was starting to form under N-rich conditions and subsequently stabilized. At about 80 min the N-signal started decreasing, which we define as the boundary between N- and Ga-rich conditions and could thus determine the critical Ga-flux relative to the N gas-flow.

In a second experiment the previous information was used to set Ga- and N-fluxes to slight N-rich conditions, while the Sb-valve was slowly opened. In this case both the Auger signals and the reflection high-energy electron diffraction pattern were observed to find the transition between crystalline and amorphous growth conditions. The sample was subsequently analyzed with Rutherford backscattering, which verified the varying Sb-composition. With the data from these two test samples subsequent films were grown with the desired bandgap of 2.2 eV suitable as photoelectrodes for photoelectrochemical water splitting application.