Etching Mask Properties of Diamond-Like Carbon Films

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1 N. New Nawachi Diamond et al. and Frontier Carbon Technology 13 Vol. 15, No MYU Tokyo NDFCT 470 Etching Mask Properties of Diamond-Like Carbon Films Norio Nawachi *, Akira Yamamoto, Takahiro Tsutsumoto and Osamu Shimakawa 1 Western Hiroshima Prefecture Industrial Research Institute Agaminami, Kure, Hiroshima , Japan 1 Kawase Machine Tech Co., Ltd Ukaicho, Fuchu, Hiroshima , Japan (Received 22 July 2004; accepted 5 November 2004) Key words: diamond-like carbon, etching, mask, MEMS The etching mask properties of diamond-like carbon (DLC) films immersed in KOH solution were investigated. In micro-electromechanical systems (MEMS) technology, anisotropic silicon etching has been used for the fabrication of microdevices. The protection (etching mask) of the silicon surface is required in the etching process. Silicon dioxide and silicon nitride have been commonly used as etching mask materials. DLC films are more chemically stable and more applicable as etching mask materials than previously used materials. In this study, DLC films were deposited on silicon substrates by three different methods, and etching experiments were carried out. DLC films deposited by radiofrequency plasma-enhanced chemical vapour deposition (RF PECVD) and ionized evaporation (IE) had a high corrosion resistance against KOH solution. DC PECVD, films, in which a lot of pinholes were observed, peeled off easily just after dipping in KOH solution. The dielectric breakdown voltages of DLC films decreased with increasing measurement temperature and became conductive over 200 C. Substrate heating over 100 C effectively prevented formation of the pinholes. 1. Introduction DLC possesses some unique properties such as high hardness and low friction. Because of these properties, there have been a lot of applications of DLC films in the tribological field. (1 3) Also, DLC films are suitable as an etching mask in semiconductor fabrication due to their chemical inertness and smooth surface. MEMS devices, such as pressure sensors and * Corresponding author: 13

2 14 New Diamond and Frontier Carbon Technology, Vol. 15, No. 1 (2005) acceleration sensors, were developed in the past. (4) Recently, the miniaturization of chemical or biochemical devices, which are called micro-total analysis systems (µtas), has been realized. (5) Wet chemical etching is a key technology for the fabrication of various MEMS. (6,7) Thus an excellent etching mask for the silicon surface is required in this process. Silicon dioxide and silicon nitride have been commonly used as etching mask materials. In this paper, we investigated the etching mask properties of DLC films deposited by three different methods. Furthermore, the influences of substrate temperature on the surface morphology and electric property of the DLC films were studied. 2. Materials and Methods The DLC films were deposited on silicon substrates by three different methods, RF PECVD, DC PECVD and IE, as shown in Fig. 1. Before loading into the chamber, the substrates were cleaned in an ultrasonic bath of acetone to remove residual organic contaminants and washed in deionised water. Prior to deposition, the chamber was evacuated, and Ar was then introduced for sputter cleaning in order to eliminate any impurities on the surfaces of the substrates. In order to examine the influences of substrate temperature on the film surfaces, DLC was deposited on a high-speed steel (SKH-51) substrate by DC PECVD. In this case, in order to improve film adhesion, an interlayer was deposited between the substrate and DLC film using tetramethylsilane (TMS). The deposition conditions are shown in Table 1. Fig. 1. Schematic diagrams of apparatuses for DLC coating, (a) RF PECVD, (b) DC PECVD and (c) ionized evaporation (IE).

3 N. Nawachi et al. 15 Table 1 Conditions for depositing DLC films Deposition method RF DC IE Substrate Si Si Si High-speed steel (SKH-51) * Gas C 6 H 6 C 6 H 6 C 6 H 6 Pressure (Pa) RF power (W) Substrate voltage (V) Substrate current (ma) Substrate temperature ( C) R.T. R.T., 100, 200, 300 R.T. Deposition time (min) Film thickness (nm) * Interlayer was formed between substrate and DLC film with tetramethylsilane (TMS). The etching experiments on DLC samples were carried out in KOH solution at 70 C. Those of SiO 2 film prepared by thermal oxidation of silicon were also carried out under the same conditions for comparison. The KOH solution has been commonly used for etching silicon wafers in the manufacture of MEMS devices. Film thickness and step height after etching were measured as shown in Fig. 2, and the etching rates of the films were estimated from these data. The surfaces of the DLC films were observed by scanning electron microscopy (SEM). In order to evaluate the effect of temperature on the electric properties of the films, dielectric breakdown voltage was measured by applying voltage between the substrate and conductive glue on the film surface at various temperatures up to 200 C as shown in Fig Results and Discussion 3.1 Etching test The surfaces of the DLC films are shown in Fig. 4. A lot of pinholes are present in the DLC films deposited by DC PECVD. These must have been formed by abnormal electric discharge during deposition. On the other hand, the surfaces of the films deposited by RF PECVD and IE were much smoother than those of the films deposited by DC PECVD. Figure 5 shows the samples after the etching test. The film deposited by DC PECVD totally peeled off just after dipping in KOH solution, as a result of its low adhesive property and it having a lot of pinholes. The gas pressure used in DC PECVD is higher than that used in the other two methods. Therefore, the amount of impurity gases such as oxygen and nitrogen must be larger, and the surface contamination of the substrate just before deposition should lower the film s adhesive property. The films deposited by RF PECVD and IE showed excellent adhesion after etching with KOH solution. However, small exfoliations are observed in the films deposited by IE and RF PECVD. The size and degree of the exfoliation are smaller for RF PECVD than for IE. It was considered that these exfoliations were formed by the formation of small pinholes,

4 16 New Diamond and Frontier Carbon Technology, Vol. 15, No. 1 (2005) Fig. 2. Procedure of etching rate measurement using surface roughness tester. *Reference surface was obtained by oxygen plasma etching of DLC which was partially covered with aluminum adhesive tape. Fig. 3. Schematic diagram of measurement of dielectric breakdown voltage. Fig. 4. SEM images of DLC film surfaces deposited by three different methods.

5 N. Nawachi et al. 17 Fig. 5. Results of etching in KOH solution. which we failed to observe in the SEM observation, and extended the peeling of films from these pinholes to the region of low film adhesion. These pinhole formations must be caused by abnormal electric discharge during deposition. RF PECVD has an advantage over IE in preventing abnormal electric discharge because the alternative current of RF PECVD neutralizes the electric charge of the DLC film surface. It is important to inhibit the abnormal discharge in order to obtain surfaces with no pinholes, which results in high durability against KOH solution. Film thicknesses and etching rates are shown in Table 2. These data were obtained using the films deposited by RF PECVD, because the number of surface defects of the films deposited by RF PECVD were less than those of the films deposited by the other two methods. The etching rate was calculated on the basis of the difference in thickness of the films between before and after etching. From no detective change in film thickness, it is obvious that the film was not etched. Hence, DLC films have a high corrosion resistance against KOH solution. SiO 2 films have been used as the etching mask for short-term etching process in KOH solution. For example, when SiO 2 films of 500 nm thickness are etched in 35 wt%koh solution at 70 C, they are durable only for approximately 2 3 h, which corresponds to less than a 200 µm etching depth of silicon. Therefore, SiO 2 films cannot be applicable to deep etching such as µm. Consequently, DLC films are excellent materials as etching masks. 3.2 Effect of temperature on morphology and electric property of film Figure 6 shows SEM images of film surfaces obtained at different deposition temperatures. The films were prepared by DC PECVD. A lot of pinholes appear in the film surface for room temperature. However, these pinholes disappear at a deposition temperature of over 100 C. Figure 7 shows dielectric breakdown voltages for these samples as a function of temperature. Generally, DLC is an insulating material. Although, the sample at room temperature shows conductivity even at low voltage. This must be due to the surface

6 18 New Diamond and Frontier Carbon Technology, Vol. 15, No. 1 (2005) Table 2 Changes in film thicknesses by etching and results of etching rates. Films Etching condition Film thickness Etching rate Etchant Temperature ( C) Time (min) change (nm) (nm/min) DLC (RF) wt%koh 120 DLC (RF) SiO wt%koh SiO wt%koh SiO wt%koh Fig. 6. SEM images of film surfaces as a function of deposition temperature. DLC films were deposited by DLC PECVD. Fig. 7. Dielectric breakdown voltage of DLC film as a function of measuring temperature. DLC films were deposited by DLC PECVD.

7 N. Nawachi et al. 19 pinholes. These pinholes are believed to be formed by abnormal electric discharge during deposition, and the substrate surface is exposed at the pinholes. Samples obtained at over 200 C substrate temperature, show insulating property at room temperature. This means that the substrate surfaces of these samples are completely covered with insulating DLC films. However, the dielectric breakdown voltages of these samples decrease with increasing temperature, and all the samples become conductive at over 200 C. The pinholes on the DLC film surfaces disappeared at over 100 C deposition temperature as mentioned above. This phenomenon must be related to the electrical properties of the DLC film. Abnormal electric discharge results from electric charging on the film surface because of the insulating property of DLC films at room temperature. However, DLC becomes conductive by heating, and this electric charge should discharge through the film at over 100 C. From these results and discussions, it is found that substrate heating is an effective way of preventing the formation of pinholes. 4. Conclusions In order to investigate their etching mask properties, DLC films were deposited on silicon substrates by three different methods, and etching experiments were carried out. Additionally, the influence of substrate temperature on the surface of DLC films was studied. The results are summarized as follows. 1) The DLC films deposited by RF PECVD and IE have a high corrosion resistance against KOH solution. 2) DC PECVD, films, in which a lot of pinholes were observed, peeled off easily just after etching in KOH solution. 3) The dielectric breakdown voltage of DLC films decreased with increasing measurement temperature and became conductive at over 200 C. 4) Substrate heating at over 100 C during deposition effectively prevented the formation of pinholes. References 1) M. Ikenaga and K. Ikenaga: J. Surf. Fin. Soc. Jpn. 53 (2002) ) T. Nakahigashi: J. Surf. Fin. Soc. Jpn. 53 (2002) ) O. Takai: New Diamond 16 (2000) 15 (in Japanese). 4) M. Esashi: J. Vac. Soc. Jpn. 45 (2002) ) S. Shoji: J. Surf. Fin. Soc. Jpn. 54 (2003) ) K. Bean: IEEE Trans. Electron Devices ED-25 (1978) ) E. Bassous: IEEE Trans. Electron Devices ED-25 (1978) 1178.

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