Accurate growth rate determination on rotating substrates using electron diffraction dynamics W. Braun, H. Möller, and Y.-H. Zhang Citation: Applied Physics Letters 74, 138 (1999); doi: 10.1063/1.122975 View online: http://dx.doi.org/10.1063/1.122975 View Table of Contents: http://scitation.aip.org/content/aip/journal/apl/74/1?ver=pdfcov Published by the AIP Publishing Articles you may be interested in Substrate preparation and low-temperature boron doped silicon growth on wafer-scale charge-coupled devices by molecular beam epitaxy J. Vac. Sci. Technol. B 20, 1170 (2002); 10.1116/1.1477200 Enabling electron diffraction as a tool for determining substrate temperature and surface morphology Appl. Phys. Lett. 79, 3065 (2001); 10.1063/1.1416477 Growth of ZnSe and ZnS films on Si(111) substrates with a nitrogen surface treatment J. Vac. Sci. Technol. B 17, 1259 (1999); 10.1116/1.590735 Reflection high-energy electron diffraction oscillations on rotating substrates J. Vac. Sci. Technol. B 17, 474 (1999); 10.1116/1.590579 Reflection high-energy electron diffraction during substrate rotation: A new dimension for in situ characterization J. Vac. Sci. Technol. B 16, 1507 (1998); 10.1116/1.589976 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: Wed, 11 Feb 2015 19:41:01 APPLIED PHYSICS LETTERS VOLUME 74, NUMBER 1 4 JANUARY 1999 Accurate growth rate determination on rotating substrates using electron diffraction dynamics W. Brauna) Center for Solid State Electronics Research and Department of Electrical Engineering, Arizona State University, Tempe, Arizona 85287-6206 H. Möller Fraunhofer-Insitut für integrierte Schaltungen-A, D-91058 Erlangen, Germany Y.-H. Zhang Center for Solid State Electronics Research and Department of Electrical Engineering, Arizona State University, Tempe, Arizona 85287-6206 ~Received 24 August 1998; accepted for publication 27 October 1998! Reflection high-energy electron diffraction oscillation frequencies are determined by measuring the width of the specular spot perpendicular to the surface during substrate rotation. Substrate rotation and data acquisition are phase locked to obtain exact rotation frequencies, allowing the inclusion of satellite peaks in the measurement. The method has a typical accuracy of well below 1% and provides a practical means to measure growth rates on rotating substrates. © 1999 American Institute of Physics. @S0003-6951~99!02301-3# Reflection high-energy electron diffraction ~RHEED! intensity oscillations are routinely used for growth rate determination in molecular beam epitaxy ~MBE!. Usually, these oscillations are measured with the substrate held at a fixed position. The accuracy of this approach is limited by the usually strong damping of the oscillations.1 Since much of this damping is due to flux nonuniformities along the surface area probed by the RHEED beam,2 measurements during rotation have the potential for greater accuracy. Attempts to measure RHEED oscillations during substrate rotation,3–5 however, have been hampered by the significant noise levels introduced by mechanical vibrations of the substrate manipulator.3 Also, the intensity of the specularly reflected spot is a very strong function of the azimuthal angle,6 requiring detectors with a very high dynamic range. In addition, substrate misorientation and wobble complicate the measurement, since the phase of the intensity oscillations is a strong function of both the azimuthal7 and the polar angle8–10 of the incident beam. Previous approaches have therefore relied on very high rotation speeds4 or spot tracking algorithms combined with numerical filtering.5 In this letter, we demonstrate a method that significantly increases the accuracy of the growth rate determination by measuring the full width at half maximum ~FWHM! of the specular spot perpendicular to the substrate during sample rotation. Our experiments indicate reliable results for substrate miscut below 0.5°, wobble below 2° and visibility of the specular spot for most of the rotation. The imaging sensor and the substrate rotation are phase locked to the same timebase, allowing us to exactly fix the rotation frequency in the measured data. We can therefore include the positions of satellite peaks in the frequency spectrum to improve the accuracy. a! Present address: Paul-Drude-Institut für Festkörperelektronik, Hausvogteiplatz 5-7, D-10117 Berlin, Germany. Electronic mail: braun@pdi-berlin.de The experiments were performed using a VG V80 MBE chamber equipped with the standard RHEED gun and the standard right angle sample manipulator. The substrate rotation was driven by a specially designed phase-locked motor synchronized to the same timebase as the charge coupled device ~CCD! camera that recorded the RHEED signal. The RHEED image processing system11 was capable of measuring at a rate of 50 Hz, leading to twice the frequency resolution compared to standard CCD-based systems. GaAs growth was monitored at a sample temperature of 560 °C measured by a Pyritte pyrometer. The measurement geometry together with a plot of the raw signal are shown in Fig. 1. The RHEED intensity is measured along a line perpendicular to the substrate surface through the center of the specular spot. During rotation, the specular spot follows a very narrow elliptical trace determined by the added contributions of substrate wobble and sample miscut. Usually, the approximation of this movement by a straight line is good enough for an accurate determination of the spot dimension along the surface normal. The line profiles plotted as a function of time are shown in the right panel of the figure. The oscillation signal is then obtained by measuring the FWHM of the peak in each trace with a subpixel-accuracy interpolation algorithm. The resulting trace of specular spot FWHM as a function of time is shown in Fig. 2. For low substrate wobble and misorienta- FIG. 1. Measurement geometry and raw signal measured from a rotating substrate. Growth oscillations are measured by determining the FWHM of the specular spot perpendicular to the substrate surface. 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: 0003-6951/99/74(1)/138/3/$15.00 138 © 1999 American Institute of Physics 209.147.144.10 On: Wed, 11 Feb 2015 19:41:01 Appl. Phys. Lett., Vol. 74, No. 1, 4 January 1999 Braun, Möller, and Zhang 139 FIG. 2. FWHM of the specular spot perpendicular to the substrate as a function of time in units of CCD pixels. Growth starts at 20 s and terminates at 80 s. FIG. 3. Frequency spectra of FWHM measurements at three different growth rates, but identical rotation frequency. The measurement time was tion, the signal is usually good enough to directly count the 180 s. oscillations. Additional experiments ~not shown! indicate that the signal-to-noise ratio of the FWHM signal perpenerror as An with the number n of satellite positions meadicular to the sample surface is much better than both the sured. At least four satellites are usually discernible, resultintensity signal integrated along the line or the FWHM signal ing in an improvement by more than a factor of 2 and a final parallel to the sample surface. This is mainly due to the accuracy of below 0.5%. For the data in Fig. 3, this resolumuch higher transfer width12 of RHEED along the beam dition corresponds to about 0.2° in the Ga cell temperature, rection compared to perpendicular to the beam. It is therefore which is getting close to the absolute temperature resolution advantageous to measure only perpendicular to the surface of MBE systems and which is certainly good enough to caliinstead of tracking the spot size in two dimensions.5 Theobrate even sensitive structures such as vertical cavity surface retical treatments of the ~01! spot size as a function of step emitting lasers. density13 indicate a strong increase in the FWHM perpenUsually, the rotation frequency is an adjustable paramdicular to the substrate with increasing step density. Qualitaeter in MBE, the case of the growth frequency being an exact tively similar results may be expected for the specular spot. multiple of the rotation frequency can therefore be avoided. It is therefore possible that the FWHM of the specular spot If the frequency spectrum is ambiguous, a change in the perpendicular to the substrate is related to the surface step rotation frequency by 32 clearly separates the peaks. The density in a much more direct way than the intensity of the method works best with the rotation frequency and the specular spot.9 growth frequency being within the same order of magnitude. In contrast to the intensity signal, the FWHM does not If the rotation frequency is too low, the effects of growth rate change by orders of magnitude in one revolution.6 The signal nonuniformity across the wafer broaden the peak. The specshows very little damping. Instead of the signal level droptra of three different measurements are shown in Fig. 4. The ping at constant noise level as in standard intensity oscillasolid line represents the Fourier spectrum of the specular tion measurements, the noise level increases at constant sigspot intensity signal without rotation, the dashed line is the nal level. Both properties together with the flat baseline of result from the integrated intensity signal along the measurethe signal in Fig. 2 make these measurements ideal candidates for Fourier transform. The transformed signals for three measurements are superimposed in Fig. 3. At a fixed rotation frequency, the growth rate was set at three different values in the measurements. The comparison of the power spectra clearly reveals the structure of the data in frequency space. The rotation frequency peaks at 0.16̄ Hz and its harmonics remain unaffected by the change in growth rate. The growth frequency exhibits a set of distinct satellites on both sides at distances of multiples of the rotation frequency. Measuring at 50 Hz sampling frequency, the FWHM of the growth frequency peak is usually very close to the limit set by the frequency–time uncertainty relationship, being approximately equal to the data point spacing in frequency space. For measurement times above 150 s, this results in a FWHM of around 1% of the absolute value for growth freFIG. 4. Comparison of the growth frequency peaks ~normalized! for three different measurement methods: ~solid line! specular spot intensity, no roquencies around 1 Hz. tation, ~dashed line! integrated intensity along the line perpendicular to the Due to the phase-locked rotation, the rotation frequency substrate through the specular spot during rotation, ~dotted line! FWHM values in the power spectrum are exact. One can therefore along perpendicular to the substrate through the specularDownloaded spot during to IP: This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the theline terms at: http://scitation.aip.org/termsconditions. measure the positions of the satellites as well, reducing the rotation. 209.147.144.10 On: Wed, 11 Feb 2015 19:41:01 140 Appl. Phys. Lett., Vol. 74, No. 1, 4 January 1999 ment line perpendicular to the substrate and the dotted line is the FWHM signal. The latter two were obtained from the same measurement using 0.25 Hz rotation. In all three cases, the growth interval was 160 s long. The FWHM of the frequency peak for the static intensity measurement is 0.027 Hz. With rotation, the width decreases to 0.021 Hz for the intensity and 0.013 Hz for the FWHM signal. The measurement based on the FWHM perpendicular to the sample surface is clearly superior, both in accuracy and also in the ratio of the growth rate peak intensity to the rotation peak intensity. The larger width for the nonrotating measurement can be explained by the strong damping of intensity oscillations.1 Much of this damping is due to growth rate nonuniformities that are strongly reduced with rotation. While it is well known that the phase of the intensity oscillations of the specular spot strongly varies with azimuthal7 as well as polar angle,8–10 which would lead to a broadening of the peak, the behavior of the specular spot FWHM oscillation phase as a function of diffraction conditions is not well known. The strong difference of the peak widths in Fig. 4 seems to imply that the FWHM of the specular spot perpendicular to the substrate is much less sensitive to these variations. Further studies are needed to clarify this point. Braun, Möller, and Zhang Part of this work was supported by a DARPA program ~Contract No. MDA972-95-1-0016! managed by G. Pomrenke. 1 J. E. Cunningham, R. N. Pathak, and W. Y. Jan, Appl. Phys. Lett. 68, 394 ~1996!. 2 J. P. A. van der Wagt, K. L. 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