Off-axis electron holographic potential mapping across AlGaAs/AlAs/GaAs heterostructures Suk Chung, Shane R. Johnson, Yong-Hang Zhang, David J. Smith, and Martha R. McCartney Citation: Journal of Applied Physics 105, 014910 (2009); doi: 10.1063/1.3062449 View online: http://dx.doi.org/10.1063/1.3062449 View Table of Contents: http://scitation.aip.org/content/aip/journal/jap/105/1?ver=pdfcov Published by the AIP Publishing Articles you may be interested in Quantitative dopant profiling of p - n junction in In Ga As ∕ Al Ga As light-emitting diode using off-axis electron holography J. Vac. Sci. Technol. B 28, C1D11 (2010); 10.1116/1.3244575 Polarization field mapping of Al 0.85 In 0.15 N / AlN / GaN heterostructure Appl. Phys. Lett. 94, 121909 (2009); 10.1063/1.3108084 Mapping the electrostatic potential across Al Ga N ∕ Al N ∕ Ga N heterostructures using electron holography Appl. Phys. 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McCartney3 1 School of Materials, Arizona State University, Tempe, Arizona 85287, USA Department of Electrical Engineering, Arizona State University, Tempe, Arizona 85287, USA 3 Department of Physics, Arizona State University, Tempe, Arizona 85287, USA 2 共Received 24 September 2008; accepted 20 November 2008; published online 13 January 2009兲 The electrostatic potential profile across AlGaAs/AlAs/GaAs heterostructures containing 1-␮m-thick n-doped 共or p-doped兲 AlGaAs layers is measured using off-axis electron holography. Simulations of the potential profiles assuming no unintentional impurities in the undoped regions of the samples show small discrepancies with experiment. Revised simulations reproduce the measurements accurately, when a p-layer with an 8.4⫻ 1011 cm−2 acceptor density is included at the buffer/substrate interface to simulate the presence of unintentional carbon impurities. © 2009 American Institute of Physics. 关DOI: 10.1063/1.3062449兴 I. INTRODUCTION AlGaAs/GaAs heterostructures have attracted intense interest for both fundamental studies in solid state physics and optoelectronic applications, such as laser diodes, lightemitting diodes, and high electron mobility transistors, ever since Esaki and Tsu1,2 suggested the possible novel properties of these heterostructures. However, impurities located at the epilayer/substrate interface have often been reported to degrade the expected performance of GaAs heterostructure devices.3,4 Studies to determine the nature of these interfacial impurities have been conducted using a range of techniques including photoreflectance spectroscopy,5,6 capacitanceversus-voltage measurements,7 deep-level transient 8 spectroscopy, and secondary ion mass spectroscopy.9,10 According to these studies, it has been shown that the presence of interfacial carbon impurities shifts the threshold voltage of field-effect transistors due to changes in band structure,3 which reduces the electron mobility and density in the channel as the thickness of the buffer layer between the substrate and active channel decreases.10 It has also been found that p-type conducting interfacial layers of carbon at the epilayer/ substrate interface cause side gating.4 As the dimensions of semiconductor devices decrease, determining the electrostatic potential distribution within deep-submicron heterostructures represents an imposing challenge. Electron holography in the electron microscope is an interferometric technique that can measure the phase change in an electron wave passing through a specimen with nanometer-scale resolution.11 Since this phase change depends on the local electrostatic potential, the technique has proven to be a powerful tool for mapping out potential variations caused by charges such as activated dopants.12 In this research, off-axis electron holography is used to determine the electrostatic potential profile across AlGaAs/AlAs/GaAs heterojunctions. The electrostatic potential drop at the epilayer/substrate interface and the corresponding sheet concentrations of charge due to interfacial impurities are determined and compared with previous studies. II. EXPERIMENTAL DETAILS Two different samples grown by molecular beam epitaxy in a VG V80H solid-source system were studied. The first sample was n-doped and consisted of a semi-insulating 共SI兲 GaAs 共001兲 substrate followed by a 100-nm-thick undoped GaAs buffer layer, an 80-nm-thick undoped AlAs layer, a n = 2.3 1000-nm-thick n-type 共NSi = 2 ⫻ 1018 cm−3, 17 −3 ⫻ 10 cm 兲 Al0.65Ga0.35As layer, and a 10-nm-thick n+ GaAs cap, as illustrated in Fig. 1. The second sample was similar to the first except that it was p-doped and consisted of a SI GaAs 共001兲 substrate followed by a 40-nm-thick undoped GaAs buffer, a 30-nm-thick undoped AlAs layer, a p = 1.5 1000-nm-thick p-type 共NBe = 2 ⫻ 1018 cm−3, 18 −3 ⫻ 10 cm 兲 Al0.65Ga0.35As layer, and a 10-nm-thick p GaAs cap. The carrier densities of the n- and p-type AlGaAs layers were determined using Hall effect measurements. Samples suitable for observation by transmission electron microscopy 共TEM兲 and electron holography were prepared using a Multiprep™ wedge-polishing apparatus a兲 Electronic mail: suk.chung@asu.edu. 0021-8979/2009/105共1兲/014910/4/$23.00 FIG. 1. Schematic of n-doped heterostructure. 105, 014910-1 © 2009 American Institute of Physics [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 209.147.144.10 On: Fri, 06 Feb 2015 17:46:26 014910-2 Chung et al. J. Appl. Phys. 105, 014910 共2009兲 FIG. 2. Annular-dark-field scanning TEM image showing cross section of p-doped heterostructure. Note the faint line of brighter contrast indicated by arrows at buffer/substrate interface. 共wedge angle of 2°兲, followed by gentle argon ion milling for a few minutes at 3.5 keV, with a current of 13 ␮A and a milling angle of ⫾5°. Off-axis electron holograms were recorded using a Philips CM200 FEG 共field-emission gun兲 TEM operated at 200 keV.13 An electrostatic biprism was inserted in the selectedarea aperture plane, and a positive voltage was applied to the biprism. This arrangement caused the vacuum or reference wave to overlap with the object wave that passes through the sample. A typical biprism voltage of 130 V resulted in an interference fringe spacing of 5 nm, and a typical primary image magnification of 15 000⫻ resulted in an effective FIG. 4. 共Color online兲 共a兲 Reconstructed phase image of n-doped heterostructure; 共b兲 comparison of simulated and experimental potential profiles along line indicated in 共a兲. Region I: n-doped AlGaAs; region II: AlAs; region III: GaAs buffer; and region IV: GaAs substrate. pixel size of 10 nm in the reconstructed phase image. An additional weak Lorentz minilens located just beneath the bore of the lower objective-lens pole-piece was used to provide an enlarged field of view of ⬃1 ␮m for holographic analysis; as compared to a smaller field of view for imaging with the normal objective lens switched on.13 During the holography observations, the samples were typically tilted by ⬃5° away from the 关110兴 zone axis about the substrate normal to minimize dynamical diffraction.14 III. RESULTS AND DISCUSSION FIG. 3. 共Color online兲 共a兲 Reconstructed amplitude image of n-doped heterostructure; 共b兲 corresponding thickness line profile. Figure 2 shows a typical cross section of the p-doped heterostructure recorded in the annular-dark-field imaging mode. The separate AlGaAs and AlAs layers are clearly visible. A faint line of brighter contrast can also be seen at the buffer/substrate interface, suggesting the presence of an unintentional delta-doped layer. Figure 3共a兲 is an amplitude mage of the n-doped heterostructure, obtained after reconstruction of the off-axis electron hologram. A line profile was taken from the region indicated by the arrow in Fig. 3共a兲, taking into account the different values for the inelastic mean-free-path of GaAs 共67 nm兲, AlAs 共77 nm兲, and Al0.65Ga0.35As 共an interpolated value of 73 nm was used兲.15 The resulting thickness profile is shown in Fig. 3共b兲, and indicates a gentle thickness increase away from the specimen edge. This image confirms a welldefined specimen geometry and indicates minimum diffracting conditions within the analyzed area. Figure 4共a兲 shows a reconstructed phase image of the [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 209.147.144.10 On: Fri, 06 Feb 2015 17:46:26 014910-3 J. Appl. Phys. 105, 014910 共2009兲 Chung et al. n-doped heterostructure. The electrostatic potential profile is extracted from the thickness and phase images in Figs. 3共a兲 and 4共a兲 using the following expression:16 ⌽= E0 + E 2␲e ⫻ V 0t = C EV 0t ␭E 2E0 + E 共1兲 where e and ␭ are the charge and wavelength of the incident electron, E is the kinetic energy, E0 is the rest energy, CE is an energy-related constant 共0.007 28 rad V−1 nm−1 for 200 keV electrons兲, and V0 is the mean inner potential. The result is shown in Fig. 4共b兲 for the line profile indicated. The sample thickness t in the analyzed area is estimated using the relationship between the incident electron-beam intensity and the reduced intensity caused by inelastic scattering.17 The electrostatic potential profile across the heterostructure is simulated using a 1D Poisson solver,18 and compared to the experimental result in Fig. 4共b兲. The experimental measurements provide the electrostatic potential profile within an arbitrary voltage offset, which is chosen so that both the experimental and simulated potential profiles are zero in the AlGaAs layer. The values for the mean inner potential difference 共⌬V0兲 used in the simulation are 共i兲 the published value of 1.9 V for the AlAs/GaAs interface15 and 共ii兲 an interpolated value of 0.7 V for the Al0.65Ga0.35As/ AlAs interface, assuming a linear relationship between ⌬V0 and composition. In comparing the experimental and simulated profiles, the change in the experimental potential is more than that predicted by the simulation in the AlAs layer. Most notably, the measured potential shows a substantial decrease in the GaAs buffer, a minimum at the buffer/substrate, and an increase in the substrate, which are not predicted by the simulation. In order to improve the agreement with experiment, the simulation is revised to include a negative electrostatic sheet charge caused by unintentional impurities at the buffer/ substrate interface. The calculated band-edge energy diagram for the n-doped sample is shown in Fig. 5共a兲, where a p-type impurity sheet with an 8.4⫻ 1011 cm−2 accepter concentration is included at the buffer/substrate interface. The electrostatic potentials for the experimental measurements and the simulations with and without the acceptor impurities are compared in Fig. 5共b兲. Further improvements between experiment and simulation are realized by adjusting ⌬V0 on each side of the AlAs layer. The revised values are 0.87 V at the AlGaAs/AlAs interface and 1.85 V at the AlAs/GaAs interface, which are reasonable when uncertainties in the electrostatic potential measurements and the alloy composition are considered. Furthermore, both the experimental profile and the simulation with impurities show a potential decrease of 0.5 V at the buffer/substrate interface relative to the constant potential in the substrate, as indicated by the arrow. This potential drop corresponds to an electric field of 3.8 ⫻ 104 V cm−1 and compares well with previously reported potential drops of 0.45V,19 and electric fields on the order of 104 V cm−1 in GaAs epilayer/GaAs substrate structures.20 The negative sheet charge can be explained by the presence of impurities on the surface of the substrate. Impurities such as carbon, silicon and oxygen at the epilayer/substrate interface have been reported in the literature,3,20 and the im- FIG. 5. 共Color online兲 Band-edge energy diagram and electrostatic potential of n-doped heterostructure; region I: n-doped AlGaAs; region II: AlAs; region III: GaAs buffer; and region IV: GaAs substrate. 共a兲 Band-edge energy simulation that includes a negative sheet charge due to impurities at buffer/ substrate interface. 共b兲 Electrostatic potential comparisons between measurement and simulations with and without impurities at buffer/substrate interface. purity concentrations have been reported to be growthcondition dependent8 and to range from a fraction to one monolayer.3 Carbon and silicon impurities can act as shallow acceptors and donors, respectively, for GaAs, while oxygen can be a deep-level impurity for nonradiative recombination centers.3,21 Reynolds and Geva10 have shown that there is a relationship between carrier depletion near the interface and net interface impurity 共关C兴-关Si兴 cm−3兲, suggesting that the amount of accumulated sheet charge is a function of 关C兴-关Si兴cm−3 at the interface. Similarly, the simulated and experimental electrostatic potentials are compared for the p-doped heterostructure. The band-edge energy diagram is shown in Fig. 6共a兲 and the electrostatic potential profile is shown in Fig. 6共b兲. The simulation with impurities again includes a sheet layer of 8.4 ⫻ 1011 cm−2 acceptors at the buffer/substrate interface. The values used for ⌬V0 are 0.7 V at the AlGaAs/AlAs interface and 1.8 V at the AlAs/GaAs interface. As before, the agreement with experiment is improved when the electrostatic potential simulation includes the presence of acceptor impurities at the buffer/substrate interface. Once again, the experiment and the simulation with impurities show a poten- [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 209.147.144.10 On: Fri, 06 Feb 2015 17:46:26 014910-4 J. Appl. Phys. 105, 014910 共2009兲 Chung et al. erostructures. Electrostatic potential drops were observed at the epilayer/substrate interface of both n- and p-doped heterostructures and were attributed to ionized carbon acceptors. The measured potential profiles in the region of the buffer/ substrate interface were accurately simulated by adding an accepter impurity layer with a sheet concentration of 8.4 ⫻ 1011 cm−2 at the buffer/substrate interface. The holography technique could also be used to determine the sheet concentration of charge for the interface states at oxide/ semiconductor interfaces. ACKNOWLEDGMENTS This work was partially supported by the Department of Energy 共Grant No. DE-FG02-04ER46168兲. We acknowledge the use of facilities in the John M. Cowley Center for High Resolution Electron Microscopy at Arizona State University. 1 L. Esaki and R. Tsu, IBM Research Internal Report No. RC-2418, 1969. L. Esaki and R. Tsu, IBM J. Res. Dev. 14, 61 共1970兲. 3 C. L. Reynolds, Jr., H. H. Vuong, and L. J. Peticolas, IEEE Trans. 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Phys. 59, 2833 共1986兲. 2 FIG. 6. 共Color online兲 Band-edge energy diagram and electrostatic potential of p-doped heterostructure; region I: p-doped AlGaAs; region II: AlAs; region III: GaAs buffer; and region IV: GaAs substrate. 共a兲 Band-edge energy simulation that includes a negative sheet charge due to impurities at buffer/ substrate interface. 共b兲 Electrostatic potential comparisons between measurement and simulations with and without impurities at buffer/substrate interface. tial decrease of 0.5 V at the buffer/substrate interface relative to the constant potential in the substrate, as indicated by the arrow. IV. CONCLUSIONS Off-axis electron holography has been used to map the electrostatic potential profile across AlGaAs/AlAs/GaAs het- [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 209.147.144.10 On: Fri, 06 Feb 2015 17:46:26