Surface Smoothing of Compound Semiconductor Substrates with Gas Cluster Ion Beams S. Houzumi, N.Toyoda, I.Yamada Laboratory of Advanced Science and Technology for Industry, Himeji Institute of Technology, 3-1-2 Kouto, Kamigori, Ako-gun, Hyogo, 678-1205 Japan Abstract. Surface smoothing by gas cluster ion beams (GCIB) was studied for compound semiconductor such as GaN and SiC. Average cluster size of Ar cluster ions was 2000atoms/cluster measured by time of flight (TOF). Since the total acceleration energy was 20keV, the energy per atom was 10eV/atom. This low-energy characteristic of gas cluster ion beams is desirable for compound semiconductors. GCIB irradiation was employed to remove the scratches of the mechanically polished SiC surface. After irradiation at acceleration energy of 15keV, the scratches was completry removed. The GaN film with initial average roughness of 4nm was also smoothed to that of 1.4nm by Ar cluster ion beams. Furthermore SiC substrates were irradiated with SF6 cluster ions. The sputtering yield of SiC with SF6 cluster ions was enhanced almost 3 times than that with Ar cluster ions. sputtering phenomena is developed by lateral sputtering effects [3]. This effect involves high sputtering yields [4] and strong surface smoothing effects. For example, surface smoothing with Ar cluster ion beams have been successfully demonstrated for CVD diamond films [5]. Also, dense energy deposition near surface is occurred in the case of gas cluster ion bombardment. When reactive gas cluster ions are employed, enhancements of chemical reactions are remarkable. In this study, Ar and SF6 cluster ion beams were irradiated to GaN and SiC surface and the surface smoothing and etching effects were studied. INTRODUCTION Compound semiconductors such as GaN and SiC are used for power device, opt-electronic device, light emitting diode (LED) [1] and high-speed semiconductors. The developments of these substrates are also enthusiastically carried out, however, grown surface is rough and it has to be polished by mechanical polishing. But these mechanical polishing easily induces scratches and subsurface damages in compound semiconductor surfaces which are not easy to recover. So, new surface smoothing method is withed that it changes into mechanical polishing. Gas Cluster Ion Beam (GCIB) is one of a candidate to realize surface smoothing without these scratches. Surface smoothing with gas cluster ion beams, which have been developed at Kyoto university. Cluster is consist of a few thousands atoms, and the energy per constituent atom of cluster is total energy divided by its cluster size. Therefore very low-energy (several eV/atom) ion beam [2] can be easily realized by employing large cluster ions. As compound semiconductor is very sensitive to damages by energetic ions, it is desirable to employ these lowenergy ion beams. When substrates surface is irradiated with GCIB, EXPERIMENT A schematic of the gas cluster ion beams apparatus for surface smoothing is shown in figure.1. This system has four vacuum chambers; source, differential pumping, ionizing and target chambers. Source chamber has a nozzle and neutral clusters are formed by supersonic expansions of high-pressure Ar and SF6 gas. To improve the vacuum pressure in ionizing chamber, differential pumping chamber was located between source and ionizing chamber. In CP680, Application of Accelerators in Research and Industry: 17th Int'l. Conference, edited by J. L. Duggan and I. L. Morgan © 2003 American Institute of Physics 0-7354-0149-7/03/$20.00 723 ionizing chamber, there are ionizer, accelerator and beam scanner. Cluster ion current was measured with a Faraday cup in the target chamber. He gas mixture was 95% in SF6, SF6 neutral beam intensity shows maximum intensity. Mass [amu] 50000 100000 150000 200000 2atm Intensity [a.u] 4atm FIGURE1. A schematic of the gas cluster ion beams apparatus for surface smoothing To measure the cluster size distribution of ion beam used for surface smoothing in this system, simple time of flight (TOF) measurements were performed. By using the scanner installed in the ionizing chamber, the actual size of the cluster ions under the irradiation condition can be measured. Pulse bias (~3kV) with 10µsec duration time was supplied on the beam scanner and ion-bunch was formed with a 1mm slit located at 5cm downstream of the scanner. Then flight times of these ions were measured from ion current at a Faraday cup located at 50cm from the scanner and stored in a digital oscilloscope. Cluster size distribution was obtained from an average of 256 repetition of time of flight measurements. Figure.2 shows cluster size distribution of Ar cluster ion beam with various gas inlet pressures (1-6atom). The acceleration energy was 20keV. The ionization energy of electron and ionization current were 100eV and 60mA, respectively. As the TOF system used here was very simple, mass resolution of TOF was quite poor. However, rough cluster size distribution can be extracted from these spectra and it was enough to ascertain the existence of cluster ions. From figure 2, the peak position and size distribution shifted to larger sizes with increasing the inlet gas pressure. When source gas pressure was 6 atm, the TOF mass spectrum was a maximum at around a size of 3000 atoms/cluster (atomic mass 120,000). As we found that the increase of ionization current caused increase of fraction of monomer ions, the ionization current was fixed at 60mA throughout this study. Ar gas is easy to form cluster beams at room temperature, since intermolecular force of Ar is strong. On the other hand, SF6 is difficult to form intense cluster beams from pure SF6 gas because SF6 molecule has many vibration modes. To produce strong SF6 cluster beams, Helium gas was mixed in SF6 gas. The role of He is to remove heat during the expansion and He itself is not incorporated in SF6 cluster beam. When 6atm 1atm 1000 2000 3000 4000 5000 Cluster size [atoms/cluster] FIGURE2. TOF spectra of Ar cluster size at different source gas pressures. Cluster size ranges from 400 to 5500 atoms/cluster. GaN and SiC were used as compound semiconductor target. GaN was deposited by hydride vapor phase epitaxy method (HVPE) [6]. Ar cluster ion beams irradiated to GaN films at normal incidence with acceleration energy of 20 keV and ion dose of 2×1016ions/cm2. After irradiation, the surface morphology of the GaN was observed with atomic force microscope (AFM, JSPM-4200, JEOL). The scanning area was 1µm×1µm. Also 3C-SiC wafers were irradiated with Ar and SF6 cluster ion beams at normal incidence. The acceleration energy and ion dose were 15keV and 7×1016 ions/cm2, respectively. After irradiation, surface morphology of the SiC was also observed with AFM (Scanning area was 8µm×8µm). When a reactive gas such as SF6 is used as a cluster source gas, enhancement of sputtering yields due to chemical reactions with target is expected. The sputtering yield was obtained from an etching depth measured with a contact depth profiler. The irradiated area was covered with a screen as a mask. To confirm the ion dose dependence of the etching depth and average roughness of SiC with Ar and SF6 cluster ion beams, SiC wafers were irradiated with Ar and SF6 cluster ion beams. The acceleration energy was 20keV and the ion dose ranged from 5×1014 ions/cm2 to 2×1016 ions/cm2. 724 acceleration energy was 20keV at normal incidence. The ion dose ranged from 5×1014 to 2×1016 ions/cm2 RESULTS AND DISCUSSIONS Figure.3 shows AFM images of GaN surface before and after irradiation with Ar cluster ion beams. Before irradiation, GaN surface was quite rough due to its columnar growth with average roughness of 4.0nm. After irradiation of 20keV Ar cluster ion beams, the average roughness was reduced to 1.4nm. It was almost one third of the initial value. Also no large grains were observed after irradiation. (a) Before irradiation, Ra=7.4nm (a) Before irradiation, Ra=4nm (b) After irradiation, Ra=0.9nm FIGURE4. AFM images of SiC surface before and after irradiation with Ar cluster ion beams. The acceleration energy was 15keV and the ion dose was 7×1016 ions/cm2 600 Total energy:20keV SiC (b) After irradiation, Ra=1.4nm FIGURE3. AFM images of GaN surface before and after irradiation with Ar cluster ion beams. The acceleration energy was 20keV and the ion dose was 2×1016ions/cm2 SF6 cluster Etching Depth [nm] 500 3C-SiC wafers were also irradiated with Ar cluster ion beams in order to remove the scratches induced by mechanical polishing. The initial surface of SiC is shown in Figure.4 (a). Before irradiation, there were many scratches on the surface. The average roughness of the SiC substrate was 7.4nm with scanning area of 8µm square. Figure.4 (b) shows the AFM images of SiC wafer after Ar cluster ion beams irradiation. When the SiC were irradiated with Ar cluster ion beam at the energy of 15 keV, the average roughness was reduced to 0.9nm and there was no scratches on its surface. As it is very difficult to remove these scratches with mechanical polishing, this scratch removal is very promising for surface finishing of compound semiconductor wafers. Figure 5 shows the ion dose dependence of etching depth of SiC with Ar and SF6 cluster ion beams. The 400 300 200 Ar cluster 100 0 0.0 0.5 1.0 1.5 16 2.0 2 Dose [ ×10 ions/cm ] FIGURE5. Ion dose dependence of the etching depth the SiC with Ar and SF6 cluster ion beams, the acceleration energy was 20keV, the ion dose ranged from 5×1014 ions/cm2 to 2×1016 ions/cm2 725 CONCLUSIONS 20 Average roughness [nm] Total energy:20keV SiC In this paper, surface smoothing effects of Ar and SF6 cluster ion beams for compound materials such as GaN and 3C-SiC were studied. In both cases, the surface roughness monotonically decreased with increasing the ion dose by 20keV Ar cluster ion beams. Scratches on SiC wafer induced by mechanical polishing were completely removed after irradiation. The sputtering yield of SiC was enhanced with SF6 cluster ions and the etching rate was almost three times higher than that of Ar cluster ions. However, it requires thicker SiC layers to realize the surface with the same roughness as that processed with Ar cluster ions. Ar and SF6 cluster ion offers various smoothing and etching methods and these are promising to apply for surface polishing of compound semiconductor wafers. 15 SF6 cluster 10 5 0 Ar cluster 0 100 200 300 400 500 Etching Depth[nm] FIGURE6. Etching depth dependence of average roughness of SiC surface with Ar and SF6 cluster ions, the acceleration energy was 20keV, the ion dose ranged from 2×1015 ions/cm2 to 5×1016 ions/cm2 REFERENCES and the average cluster size was 2000atoms/ion. From Figure 5, the etching depth increased monotonically with increasing ion doses. When irradiation dose of Ar cluster ion was 2×1016 ions/cm2, etching depth was about 190nm. On the other hand, when SF6 cluster ion beams were irradiated with the same ion dose, sputtering depth of SiC was about 620nm. It was almost three times higher than that of Ar cluster ion beams. Since SF6 is a reactive gas, enhancement of sputtering yields due to chemical reactions with SiC was significant. These enhancements of sputtering yields with SF6 were also observed in Si and W. Figure 6 shows etching depth dependence of average roughness of SiC surface after etching experiment with Ar and SF6 cluster ions shown in figure 5. In the case of Ar irradiation, the average roughness of SiC decreased monotonically with increasing the etching depth from the initial value of 15.7nm to 2.3nm at an etching depth of 186nm. In the case of SF6 irradiation, the average roughness decreased from 15.7nm to 3.2nm at etching depth of 450nm. From figure 5, SF6 cluster etches almost three times thicker SiC than Ar at the same ion dose. It means that SF6 cluster ion requires thicker SiC layers to smooth the surface, and the smoothing effect is weaker than that of Ar cluster ion beams. From these results, surface smoothing of compound semiconductor was demonstrated with Ar and SF6 cluster ion beams, and it is candidate for surface finishing process of these substrates. 1. S. Nakamura, T. Mukai, M. 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