DEPOSITION OF Al 2 O 3 ON CERAMIC SUBSTRATES BY PECVD METHOD. Lucie Špirková a Vlastimil Brožek a Jean Durand b
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1 DEPOSITION OF Al 2 O 3 ON CERAMIC SUBSTRATES BY PECVD METHOD Lucie Špirková a Vlastimil Brožek a Jean Durand b a) Institute of Chemical Technology, Prague, Czech Republic b) Laboratoire des Matériaux et Procédés Membranaires (CNRS UMR 9987), Ecole National Supérieure de Chimie, Montpellier, France Abstract Low temperature deposition of aluminum oxide films using a plasma enhanced metalorganic chemical vapor deposition technique is described. The plasma was generated by a 40kHz RF. A single molecular source reagent trimethylaluminum, Al(CH 3 ) 3 was carry away into the reacting chamber by He-carrier gas. The films were deposited over the temperature range C. Films were deposited on silicon wafers and porous ceramic plates. The thickness, structure and surface morphology were observed using scanning electron microscopy. 1 INTRODUCTION Aluminum oxide offers high radiation resistance [1], high thermal conductivity and very low permeability of alkali ions and other impurities [2]. The chemical stability against almost all known media makes it nearly ideal material for wear-protective coating on cutting tools for nonaluminum workpieces. Thin films-layers of Al 2 O 3 have been extensively used in optical and electronic industries, as protective films for metal reflectors, laser mirrors, masks against impurities, and as passivation layers in metal/oxide/semiconductor devices [3]. Aluminum oxide films on porous ceramic substrates can find an application as a top separating layers in membranes for ultrafiltration. In such applications, aluminum oxide films have been prepared by means of chemical vapor deposition (CVD) and physical vapor deposition (PVD) methods [4-6]. High-temperature CVD processes often cause unwanted thermal strain and diffusion problems. PVD processes, such as evaporation or sputtering, do not provide good coverage of surface steps, and are therefore not suitable for multilevel devices having complicated surfaces morphology. A considerable interest has been taken in low-temperature deposition process having good step coverage. Plasma-enhanced chemical vapor deposition (PECVD) process satisfies the above requirements, although it has some limitations [7]. Recently several researches adopted the low-temperature PECVD method for the preparation of aluminum oxide films using trimethylaluminum (TMA) source [8-10]. In the present work, aluminum oxide films were deposited on two types of supports: commercial silicon wafers and ceramic plates prepared by thermal spraying of gray alumina Al 2 O 3 / 3%wt TiO 2.
2 2 EXPERIMENTAL 2.1 Apparatus The apparatus for the plasma-enhanced chemical vapor deposition of aluminum oxide is shown in Fig.1. Pirani gauge gas manifold aluminum electrodes 40 khz generator TMA precursor reservoir sample support rotary pump heating and temperature controller sample holder He N 2 O Fig.1 Scheme of the reacting apparatus It consists of a reaction tube chamber made of glass, an RF. generator (40 khz), a pumping system, and a gas manifold. The reactor is furnished by two aluminum electrode plates. In contrast to high frequency discharge (13.56, 40 or 80 MHz) in previous works [7,8], the excitation frequency of 40 khz produces plasma with a small potential drop. This frequency corresponds to a higher growth rate of the deposited layer. The support holder, aluminum disk, was located in the middle of the reactor, about 2 cm under the bottom of the electrodes. During the deposition, the temperature of the substrate was maintained with a thermocouple in the range of C. The apparatus is evacuated with a rotary oil pump, the pressure in the reactor is monitored with a Pirani gauge. The precursor trimethylaluminum TMA was kept in the reservoir in an inert atmosphere at the temperature range C, in order to avoid condensation there. The gas flow is regulated with needle valves. N 2 O was used as plasma ionization gas. The precursor is introduced into the reactor in a carrier gas-he stream. The pressure conditions were
3 chosen as follows: p(he,tma) = 0.1 mbar, p(he,n 2 O,TMA) = 0.5 mbar. The deposition time was min and the thickness of the layers varied from 100 nm to 2 µm. 2.2 Substrates Silicon wafers (30x10x0.7 mm) and alumina ceramic substrates (30x10x1.5 mm) were used. Commercial silicon is a readily available material which has a smooth surface and, owing to its infrared transparency, allows additional characterization of the deposited films. For some comparisons, rough alumina ceramic substrates prepared by thermal spraying of gray alumina (Al 2 O 3 / 3%wt TiO 2 ) powder (feedstock size in the range µm), were used. The porosity of the second type of substrates varies from 7 12 %, and the mean pore size is about 10 µm. 2.3 Characterization of the deposited films For the SEM analysis, samples about 5x5 mm were prepared and sputtered with Pt. The samples were characterized using scanning electron microscopy (SEM) to determine the morphology, thickness and grow rate of the layers. The chemical composition and carbon content were measured with an energy dispersion X-rays spectrometer (EDX). The layers were not sufficiently thick to determine the crystal structure by X-ray diffraction. 3 RESULTS The chemical composition of the deposited samples is shown in Fig. 2. EDX analysis proved that the samples contain no carbon. It can be, therefore, assumed a complete decomposition of organic precursor in the plasma medium. Fig.2. EDX analysis of Al 2 O 3 film on ceramic substrate On the silicon substrates, smooth and uniform aluminum oxide films were deposited. For deposition on substrates at the low temperature ( C), compact films with a grow rate of maximum 20 nm min -1 were obtained. The free surface is covered with a ball-shaped structure, growing out of the µm at the surface (Fig.3). After cooling down, a cracking occurs and the layer starts to detach from the substrate. The higher temperature of the substrate, the larger the grains of the deposits.
4 Fig.3 The free surface covered with a ball-shaped structure. After cooling down, a cracking occurs and the layer starts to detach from the substrate. Fig.4 For the substrate temperature 250 C, columnar structure with no cracks. Fig.5 Structural features of 1,5 µm in diameter with a different shapes are on free surface of ceramic substrate. Fig.6 Layer formation on the surface overlaps existing narrow pores For the substrate temperature between C, the structure becomes columnar, no cracks appear after cooling down, and films are more adherent (Fig.4). There is a strong decrease of the grow rate for the substrate temperature over 350 C. In the second case of ceramic substrate, the influence of the porous, rough ceramic surface on the film formation can be observed. The surface is, however, entirely covered by the deposits, but structural features of some µm in diameter with a different shapes are on free surface. It can be supposed, that in these places, the
5 nucleation and grain growth were preferential, due to the presence of impurities (fence), in the feedstock gray alumina powder (Fig.5). The nucleation starts on an active centers in the form of islets, which gradually enlarge and when they reach up to 100 µm, they start to coalescent with each other. Fig.6 shows that a layer formation on the surface overlaps existing narrow pores (in our case the pore width is 1 µm). 4 CONCLUSION Homogenous aluminum oxide films were deposited at by the plasma enhanced chemical vapor deposition. The temperature of the substrate dominates the growth rate and the grain size of deposits. The morphology observations indicate that to obtain adhesive, granulated compact films, at the frequency of RF 40 khz, the substrate temperature should be between C. Impurities on the ceramic surface probably lead to the formation of deposits with a large roughness. 5 REFERENCES [1] Zaininger K.H., Waxman A.S., IEEE Trans. Electron Devices, ED-16, 1969, p.333 [2] Abbott D.A. and Kamins T.I., Solid State Electron, 13, 1970, s.565 [3] Mansour S. Al-Robaee and Ghanashyam Krishna M., Subanna G.N., Narasimha Rao K. and Mohan S. Properties of Al 2 O 3 films prepared by argon ion assisted deposition, J.Mater. Res., Vol.9, No. 10, Oct 1994 [4] Fournier J., DeSisto W., Brusasco R., Sosnowski M., Kershaw R., Baglio J., Dwight K., Wold A., Mater. Res. Bull., 23, 1988, s.31 [5] Maruyama T., Nakai T., Appl. Phys. Lett. 58 (19), 1991, s.2079 [6] Kumagai H., Toyoda K., Matsumoto M., Obara M., Jpn. J. Appl.Phys. 32, 1993, s.6137 [7] Yong-Chun Kim, Hyung-Ho Park, John S. Chun and Won-Jong Lee, Thin Solid Films, 237, 1994, s.57 [8] Wang H.L., Lin C.H., Hon M.H. The dependence of hardness on the density of amorphous alumina thin films by PECVD, Thin Solid Films 310, 1997, s.260 [9] Meiners L.G., Thin Solid Films, 113, 1984, [10] Catherine Y., Talebian A., J. Electron Mat., 17, 1970, 127
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