Thin Solid Films 367 (2000) 290±294 www.elsevier.com/locate/tsf MBE growth of planar microcavities with distributed Bragg re¯ectors K. ReginÂski*, J. Muszalski, M. Bugajski, T. Ochalski, J.M. Kubica, M. Zbroszczyk, J. KaÎtcki, J. Ratajczak Institute of Electron Technology, Warsaw, Poland Abstract We discuss some problems of molecular beam technology (MBE) technology of planar microcavities based on GaAs, AlGaAs and InGaAs compounds. This technology needs speci®c methods of in situ control and postgrowth characterization. One of the crucial problems is that of controlling the substrate temperature and the growth rate with very high accuracy. We demonstrate the usefulness of substrate temperature oscillations observed by infrared pyrometry for both the temperature and the growth rate control. For studying the perfection of layers and interfaces the cross-sectional transmission electron microscopy has been used. To optimize the optical characteristics of the microcavities, several experimental methods have been applied. The Bragg re¯ectors were investigated by optical re¯ectivity. For selective excitation of a quantum well (QW) in a cavity active layer, the Ti-sapphire tuneable laser have been used. The ®ne tuning between the QW emission and the cavity Fabry±Perot resonance has been investigated by photoluminescence for varying temperature of the sample. q 2000 Elsevier Science S.A. All rights reserved. Keywords: Molecular beam technology growth of Bragg re¯ectors; Planar microcavities; Vertical cavity surface emitting lasers 1. Introduction Vertical cavity surface emitting lasers (VCSELs) have been attracting much attention in recent years and a lot of different devices have been demonstrated by using various growth techniques [1±3]. The laser cavity of VCSEL is usually constructed normal to the substrate plane by stacking multilayer ®lms including an active region and two dielectric mirrors. Such a structure forms a Fabry±Perot cavity resonator. A dielectric mirror can be formed with a periodic stack of quarter wavelength thick layers of alternating high and low refractive index material. Such a mirror is referred to as a distributed Bragg re¯ector (DBR). The dielectric layers can be semiconductor layers deposited via molecular beam epitaxy (MBE) growth. The active region consists usually of a layer of GaAs of the thickness of one wavelength or half a wavelength and of one or several quantum wells (QWs) of InGaAs (in our case In0.20Ga0.80As has been applied). The quantum wells are typically situated in the antinodes of a standing electromagnetic wave [4]. An example of such a structure is presented in Fig. 1. This is the whole VCSEL structure designed for l 1000 nm emission. A l-cavity is made of GaAs and contains in the center one QW made of In0.20Ga0.80As. * Corresponding author. 32/46. Lotnikow Avenue, PL-02-668 Warsaw, Poland. Tel.: 1 48-22-548-7920; fax: 1 48-22-847-0631. E-mail address: [email protected] (K. ReginÂski) The procedure of designing the MBE process for growing the VCSEL structure comprises two classes of problems. The ®rst one is connected with growing the materials of high quality for all parts of the structure. This optimization concerns GaAs, Al(Ga)As, and InGaAs compounds. The problem is typical for MBE technology and can be solved by standard methods: We optimize the MBE technology by testing different substrate temperatures, different growth rates, and different arsenic to metal ratios. Similarly, the problem of smoothness of interfaces is solved typically by comparing the interfaces made with and without the growth stopping. The second group of problems is characteristic of the VCSEL structure. Optimization of such a structure requires the precise tuning of its main parts ± Bragg re¯ectors, GaAs cavity and QWs. From theoretical modeling as well as from test processes it follows that the structure perfection is very sensitive to variation in thickness of the separate layers and their composition [4]. The required accuracy can hardly be achieved without additional non-standard internal control in the MBE system. Thus, besides the careful calibration of the growth rate and composition, some non-standard methods of internal control should be applied. Moreover, to test the grown structures, we should combine several methods of postgrowth characterization. The experimental works should also be combined with theoretical calculations of optical properties of separate DBRs and the whole micro- 0040-6090/00/$ - see front matter q 2000 Elsevier Science S.A. All rights reserved. PII: S00 40-6090(00)0069 0-8 K. ReginÂski et al. / Thin Solid Films 367 (2000) 290±294 cavities (theoretical re¯ectivity spectra and emission characteristics). 2. Precision requirements The optimization of the microcavity requires proper tuning of the wavelength of radiation emitted from the active region, the peak re¯ectivity of the DBRs, and the cavity resonance. It is the reason why the structure performance is very sensitive to variations in thickness of layers and their compositions. The wavelength of radiation from the QW depends on both the composition and thickness. The re¯ectivity of DBRs in case of GaAs/AlAs re¯ectors depends on the layer thickness in the mirrors. Similarly, the position of the cavity resonance depends on the thickness of the spacer layers between the mirrors and the QWs region and the phase of the re¯ection from the mirrors. Thus, the optimal growth of the structure requires simultaneous alignment of all three features. However, some variation of those parameters can be tolerated depending on how much variation in threshold and ef®ciency is acceptable from device to device. From theoretical considerations it follows that even a 10% error in layer thickness does not signi®cantly degrade the peak re¯ectivity, but in this case the stop band is shifted in wavelength [5]. Also of interest is the effect of having one layer in the DBR thinner than a quarter wavelength and one thicker. The result of the offsetting thickness variations is to decrease slightly the peak re¯ectivity of the mirror. Thus, the goal in growing the mirrors for a VCSEL is to get the layers each approximately a quarter wavelength thick and to get the re¯ection band centered at the right wavelength. If the layers slightly differ from a quarter wavelength, it is not so important as long as the re¯ection band is situated in the right place. The position of the cavity resonance will ultimately determine the lasing wavelength. From theoretical considerations it follows that in a properly fabricated laser Fig. 1. Layer structure of a vertical cavity surface emitting laser designed for l 1000 nm emission. 291 structure the wavelength of the re¯ectivity peak may be shifted by ^2%, or each layer thickness may vary by ^2%. It means that the accuracy of the control of gallium and aluminium ¯uxes should be of the order of 2%. The ®nal issue to consider is the effect that a change in layer thickness and composition has on the wavelength emitted from the active region. For an InGaAs quantum well there are two effects to account for: a change in band gap with composition and a change in electron and hole con®nement energies with well width. From simple calculations it follows that even an error in Ga ¯ux of 5% causes negligible change in the transition energy since the increased con®nement energy is compensated by the decreased band gap. The same calculations for a 5% error in the In ¯ux show a wavelength shift one order of magnitude greater. Whereas a small change in the Ga ¯ux will cause no noticeable shift in the transition energy, the In ¯ux should be extremely accurate. In reality, it is very dif®cult to obtain stabilization of the ¯ux better than 2% without a realtime control of the growth rate in the MBE system. 3. Experimental set-up and growth of the structures The growth processes reported in this study have been performed by Elemental Source MBE technique on RIBER 32P machine equipped with ABN 135L evaporation cells. Certain details of the control system installed in the growth chamber of this machine are presented in Fig. 2. The molecular ¯uxes were measured by a Bayard±Alpert gauge mounted on the sample manipulator. The manipulator could be rotated so as to place the Bayard±Alpert gauge at Fig. 2. Details of the control system installed in the growth chamber of RIBER 32P MBE machine. 292 K. ReginÂski et al. / Thin Solid Films 367 (2000) 290±294 the standard position of the substrate. Thus the gauge could measure the beam equivalent pressure (BEP) of the As4, Ga, Al, and In beams. For monitoring the state of the crystal surface during the growth the re¯ection high energy electron diffraction (RHEED) system with a 10 keV electron gun was used. The RHEED patterns were registered by CCD camera and then processed in real-time and recorded by a computer acquisition system. This system consists of a personal computer equipped with a frame grabber, two monitors, and a high resolution laser printer. The RHEED pictures could be processed by a specially written computer program and stored on a hard disc for further reference. The system also enables us to register RHEED intensity oscillations and, as a result, to determine the growth rate of a layer. The substrate temperature was measured with an thermocouple and simultaneously with an IRCON Modline Plus pyrometer. This particular model of pyrometer is specially designed to measure the GaAs surface temperature by monitoring the radiation emitted in a narrow range of wavelengths (0.940 ^ 0.03 mm) which is shorter than the band edge of GaAs (but longer then AlxGa12xAs, x . 0:25) at the temperatures which are of interest for MBE (400±7508C). The pyrometer is connected with a computer system enabling registration the pyrometric temperature as a function of time. During the growth of the structure, even if the temperature registered by a thermocouple is constant, the pyrometric temperature oscillates in time. The source of those apparent temperature oscillations is the interference of the radiation emitted from the substrate and the radiation re¯ected at the underlying layer/grown layer and grown layer/vacuum interfaces. The phase information and the period of oscillations provide information on the actual growth rate, whereas the mean value of the pyrometer readout correlates with the true substrate temperature. Analysis of the oscillation curve after the growth gives as direct information about thickness of all the layers in the grown structure. Thus, the interference pyrometry offers a convenient alternative to a standard laser re¯ectometry when it is necessary to control growth rate of layers with high precision. More details about this control system one can ®nd in [7]. The calibration of the growth rate of the layers was performed in several steps. The preliminary calibration has been performed by combining two methods. First, the necessary values of temperatures of effusion cells were found by using temperature±¯ux calibration curves and well known formulae for converting BEP into absolute values of ¯uxes [6]. Next, RHEED intensity oscillations were measured during the growth processes of all the semiconductor compounds applied in the structure. The results of the measurements gave some corrections into the values of effusion cell temperatures. The ultimate precision of the growth rate calibration was achieved during the test growth of the structures by using the system of registering the apparent substrate temperature oscillations. It enabled to control the growth rate of the individual layers with accuracy about 1%. As an example, a pyrometer readout during the MBE growth of the test VCSEL structure is shown in Fig. 3. In a series of processes the separate elements of the VCSEL structure as well as the whole VCSELs were grown. The VCSEL structures were designed for l 1000 nm emission. They consisted of two Bragg re¯ectors composed of 14.5 and 23.5 pairs of AlAs/GaAs quarter wavelength layers. A l-cavity was made of GaAs and contained in the center a QW made of In0.2Ga0.8As. This structure is presented in Fig. 1. The growth has been performed on the GaAs p2substrate of (001) orientation. The optimized growth temperatures were as follows: the GaAs:Be buffer layer was grown at 5908C; the AlAs/GaAs Bragg re¯ectors, GaAs cavities and In0.2Ga0.8As QW were grown at constant temperature 5208C. The growth rate for GaAs and AlAs was 1 mm/h and that for AlGaAs was 2 mm/h. The background pressure during the growth was 5 £ 10 8 Torr. The whole process was performed without any stopping. During the growth of the main structure, the substrate temperature shown by a thermocouple was kept constant. The pyrometer readout shown in Fig. 3 demonstrates that this method of regulation leads to the really good thermal stabilization of the substrate. 4. Postgrowth characterization The process of optimizing the technology comprised postgrowth characterization of the separate Bragg re¯ectors, the microcavities, and the complete VCSEL structures. Cross-sectional transmission electron microscopy (XTEM) has been used to observe the perfection of layers and interfaces. Cross-sectional specimens were prepared by the method described in [8]. The specimens were studied in a JEM 200CX (200 kV) microscope. A XTEM micrographs of the structure consisting of Bragg re¯ectors, l-cavity and In0.2Ga0.8As QW are presented in Figs. 4 and 5. Whole the structure is visible in Fig. 4. The interfaces between separate layers are sharp and the periodicity of the AlAs/GaAs layers Fig. 3. Pyrometer readout during the MBE growth of the test structure of a vertical cavity surface emitting laser. K. ReginÂski et al. / Thin Solid Films 367 (2000) 290±294 293 Fig. 4. Transmission electron microscopy micrograph of the laser l-cavity consisting of Bragg re¯ectors, GaAs region, and In0.2Ga0.8As quantum well. is in a good accordance with the project. The region of the In0.2Ga0.8As QW is presented in Fig. 5. The interfaces between QW and cavity as well as those between the cavity and the Bragg re¯ectors layers are straight and sharp. No defects in the structure are visible. Optical properties of grown structures were investigated by optical re¯ectivity and photoluminescence (PL). The re¯ectivity spectra were measured in a system by using a halogen lamp as a source of incident white light. After re¯ection the relevant wavelength is selected by monochromator and registered by Ge detector. Fig. 6 shows a typical re¯ectance spectrum measured from the structure consisting of Bragg re¯ectors, l-cavity and In0.2Ga0.8As QW. A re¯ectance spectrum for a similar structure, but with l/2-cavity, is shown in Fig. 7. A re¯ectance spectrum for the whole VCSEL structure is presented in Fig. 8. The measured spectra are similar to those calculated for ideal structures and exhibit the cavity resonance centered in the high re¯ectivity band of the Bragg re¯ectors. All the spectra exhibit broad stop bands where the plot is almost ¯at. The re¯ectivity within those frequency intervals attains nearly 100%. The stop bands are bounded by deep minima which also testi®es to the good quality of DBRs. PL measurements give us important information about the InGaAs quantum wells. To excite the quantum well, a Fig. 5. Transmission electron microscopy micrograph of the central part of the laser l-cavity. The region of In0.2Ga0.8As quantum well is shown in detail. Fig. 6. Re¯ectance spectrum and photoluminescence from the structure consisting of Bragg re¯ectors, l-cavity and In0.2Ga0.8As quantum well. Ti-sapphire tuneable laser has been used. Depending on the size of the cavity we observed either an enhancement or suppression of the coupling of 1e±1hh electronic dipole transitions into the resonant Fabry±Perot mode of the planar microcavity structure. The structures were excited with a beam perpendicular to its surface. The emission was registered either from the edge of the structure (in plane PL) or in the direction perpendicular to its surface. The emission from the edge does not show any modi®cations (comparing with a separate QW) and can be treated as a reference. The emission from the surface shows the resonance with a Fabry±Perot resonator. The large amplitude of this signal can be regarded as an evidence of good tuning between the wavelength emitted from the quantum well and the cavity resonance. Some examples of PL measurements are shown in Figs. 6 and 7. Fig. 6 shows a typical PL spectrum measured from the Fig. 7. Re¯ectance spectrum and photoluminescence from the structure consisting of Bragg re¯ectors, l/2-cavity and In0.2Ga0.8As quantum well. PL, photoluminescence perpendicular to the Bragg re¯ector; PL in plane, photoluminescence from the edge of the structure. 294 K. ReginÂski et al. / Thin Solid Films 367 (2000) 290±294 This type of measurements enabled us to accelerate the procedure of designing and testing the laser structures. 5. Conclusions Fig. 8. Re¯ectance spectrum from a vertical cavity surface emitting laser structure of l-type with an In0.2Ga0.8As quantum well. structure consisting of Bragg re¯ectors, l-cavity and In0.2Ga0.8As QW. The narrow PL peak corresponds to the case of good tuning. The PL spectra for a similar structure, but with l/2-cavity, are shown in Fig. 7. Both the types of registration of photoluminescence signal, from the edge (denoted as PL in plane) and from the surface (denoted as PL), are presented. The ®ne tuning between the QW emission and the cavity Fabry±Perot resonance has also been investigated by PL for varying temperature of the sample. Even when the whole system is not well tuned we can test the structure by registering luminescence as a function of temperature. By changing the temperature we can shift the frequency of the wave emitted from the QW and achieve the resonance for a certain temperature. An example of such measurements is presented in Fig. 9. The tested structure consisted of Bragg re¯ectors, l-cavity and In0.2Ga0.8As quantum well. Applying several methods of in situ control and combining selected methods of postgrowth characterization we have developed the MBE technology of growing the VCSEL structures. We have demonstrated that for reproducible growth of microcavities and VCSELs by MBE, the growth rate of individual layers has to be controlled with accuracy better than 2%. To achieve this accuracy we have applied a precise procedure of preliminary calibration combined with registering the pyrometric temperature oscillations. We have shown that the interference pyrometry offers a convenient alternative to a standard laser refractometry when it is necessary to control the growth rate of layers with high precision. By using the above described methods we have grown a number of microcavities and VCSEL structures of good quality con®rmed by transmission electron microscopy, photoluminescence, and optical re¯ectivity. The structures have proper characteristics of the Bragg re¯ectors and the quantum well emission wavelength precisely tuned to the cavity resonance. Acknowledgements This work has been supported by the State Committee for Scienti®c Research (Poland) under Contract Nos. PBZ 28.11/P7 and 8.T11B.064.14. References Fig. 9. Photoluminescence spectra for varying temperature of the sample. The structure consists of Bragg re¯ectors, l-cavity and In0.2Ga0.8As quantum well. [1] T. Baba, T. Hamano, F. Koyama, K. Iga, IEEE, J. Quantum Electron. 27 (1991) 1347. [2] C.J. Chang-Hasnain, in: G.P. Agrawal (Ed.), Semiconductor Lasers; Past, Present, and Future, AIP Press, Woodbury, 1995, p. 145. [3] L.A. Coldren, E.R. Hegblom, Y.A. Akulova, J. Ko, E.M. Strzelecka, S.Y. Hu, VCSELs in 98: What we have and what we can expect, in: K.D. Choquette, R.A. Morgan (Eds.), Vertical Cavity Surface Emitting Lasers II, Proceedings of SPIE, Vol. 3286, 1998, pp. 2±16. [4] T.E. Sale, Vertical Cavity Surface Emitting Lasers, Research Studies Press, Taunton (1995) 55. [5] R.S. Geels. PhD thesis, University of California, Santa Barbara, 1991. [6] G.J. Davies, D. Williams, in: E.H.C. Parker (Ed.), The Technology and Physics of Molecular Beam Epitaxy, Plenum, New York, 1985, p. 38. [7] J. Muszalski, Thin Solid Films (this issue) p. 299. [8] J. Katcki, J. Ratajczak, A. Malag, M. Piskorski, in: A.G. Cullis, A. Staton-Bevan (Eds.), Microscopy of Semiconducting Materials, IOP, Bristol, 1995, p. 273.
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