Thin Solid Films 443 (2003) 115–119 Deposition of permalloy films by filtered cathodic vacuum arc J.S. Chen1, S.P. Lau*, Y.B. Zhang, Z. Sun, B.K. Tay, C.Q. Sun Ion Beam Processing Laboratory, School of Electrical and Electronic Engineering, Nanyang Avenue, Nanyang Technological University, Singapore 639798, Singapore Received 11 February 2003; received in revised form 14 May 2003; accepted 16 July 2003 Abstract The filtered cathodic vacuum arc technique was employed to deposit magnetic films such as FeNi on silicon substrate. Using the normal cathode design, tetrahedral amorphous carbon and metals films can be deposited. If a magnetic target is used, the arc spot always preferably moves to the edge of the target and then extinguishes. Therefore, the arc is not stable and no film can be deposited. A cathode was designed to obtain stable and continuous arc and uniform erosion pattern. The atomic force microscopy, grazing X-ray diffraction and vibrating sample magnetometry were used to characterize the morphological, structural and magnetic properties of the FeNi film. When the film deposited at substrate bias of y100 V, it exhibits a square magnetization–hysteresis loop, the lowest coercivity and the highest saturated magnetization among all the investigated samples, which may be related to its good surface roughness and crystallinity. 䊚 2003 Elsevier B.V. All rights reserved. Keywords: Permalloy; Filtered cathodic vacuum arc; Magnetic properties 1. Introduction For many years there has been considerable interest in producing films of magnetic materials because of their many exclusive applications such as magnetic recording, microactuation and sensors and so on. Many techniques have been employed to synthesize the magnetic films with varying amounts of success, which include evaporation, sputtering, pulsed laser deposition, and molecular beam epitaxy w1–3x. Among them, the evaporation and sputtering are predominant in industrial application because of their economy and simplicity. But the need for new, high performance materials in magnetic recording entails the development of a new deposition technology for magnetic films. It is well known that cathodic vacuum arc technology has proven to be a very promising method for ultrathin film deposition. It offers several advantages over evaporation and *Corresponding author. Present address: Data Storage Institute, 5 Engineering Drive 1, NUS, Singapore 117608, Singapore. Tel.: q6567906439; fax: q65-67933318. E-mail addresses: esplau@ntu.edu.sg (S.P. Lau), chen_jingsheng@dsi.a-star.edu.sg (S.P. Lau). 1 Present address: Data Storage Institute, 5 Engineering Drive 1, NUS, Singapore 117608. sputtering, and the principal advantages are the high percentage of ions in the emitted flux (approx. 100%), high kinetic energy of these ions (20–200 eV) w4,5x. In the present time, it has been in wide-scale industrial use for producing wear protective coatings of TiN and related materials on cutting and forming tools, as well as decorative coatings on plumbing fixture and jewelry. Adding a magnetized torus macroparticle filter the highly tetrahedrcally bonded amorphous carbon films can be synthesized with high deposition rate (5 nmys) at room temperature w6x. The filtered cathodic vacuum arc (FCVA) technique has also been used for depositing optical thin films of metal oxides (TiO2 and Al2O3) and semiconducting thin films (amorphous Si and SnO2) w7–9x. To our knowledge, however, no paper has been reported on the deposition of magnetic films by FCVA technique yet. In this paper, the FCVA technique was used to deposit FeNi films on Si substrate. A modified cathode design for depositing magnetic films was presented. 2. Movement of cathode arc spot and cathode design The typical FCVA system has been described elsewhere w10x. Generally, a conductive target mounted on 0040-6090/03/$ - see front matter 䊚 2003 Elsevier B.V. All rights reserved. doi:10.1016/S0040-6090(03)01031-9 116 J.S. Chen et al. / Thin Solid Films 443 (2003) 115–119 Fig. 1. The schematic diagrams of cathode (a) original and (b) modified design. water-cooled copper block was used as a cathode as shown in Fig. 1a. A tube-shaped stainless steel around the outer of cathode was used as a shield to avoid straying arcing and the space between them was approximately 2–3 mm. The cathodic arc is triggered with a graphite electrode touching the cathode surface at an initial background pressure of approximately 10y6 Torr and the cathode is continuously water-cooled from the back. The plasma beam produced by the cathode spots passes through an off-plane double-bend macroparticles filter into the deposition chamber w11x. This type of filter bend has many advantages over the single bend, for example, higher ion density, higher plasma transport efficiency and significant reduction of macroparticles. The anode is grounded and the shield and the bend are under floating potential. The substrate can be biased up to negative 400 V. In such a cathode design, the arc spot on the surface of magnetic materials moves away from the center to the edge of the cathode after igniting the arc in the center, and then the arc either sustains for a short time (mostly less than a minute) or extinguishes immediately. This is quite different from that of the Ti and Cu as a cathode target. The behavior of the arc spot on the surface of magnetic targets does not change even if the filtering coils are not energized. It is well known that the cathode spots apparently move randomly over the cathode surface (Ti, Cu, Al, etc.) in the absence of a magnetic field, but in the presence of a magnetic field they have a direct velocity in the yJ=B direction, a phenomenon known as ‘retrograde’ motion. At present, most investigations on vacuum arc spot dynamics were mainly focused on high current vacuum arc because of its application for commercial vacuum circuit breakers. Siemorth et al. have shown that the cathode spot at high current should be considered as a multilevel organized self-similar structure w11x. Sherman et al. w12x have investigated the influence of self-generated magnetic field on cathode arc spots movement for copper electrode at high current vacuum arc (2.7–6.9 kA), namely, the influence of the magnetic field generated by other vacuum arc spots on a vacuum arc. According to the experimental results they derived a relationship between the retrograde spot velocity (V) and magnetic flux density (B), namely VsKØB, where K is the coefficient depending on the cathode materials and is independent of B. It has been generally believed that the arc current self-generated magnetic field is a major factor that governs the dynamics of arc spot in high-current vacuum arc. However, it is believed that there is only a single cathode spot with 10 mm in diameter in the low current vacuum arc (approx. 100 A) w13x. For the arc spots on the Ti and Cu cathodes there is no or little external force imposed on them, so it moves randomly around the surface of the cathode. The behavior of arc spot on magnetic materials can be interpreted as follows: the vacuum current is considered as a wire with current flowing. According to Ampere’s law, vacuum arc current generates an azimuthal magnetic field that can induce magnetization of magnetic materials and then produce a magnetic field. The magnetic field produced is due to the magnetization of magnetic materials, which imposes on the arc spot once it moves and makes a retrograde motion, namely, the cathode arc spot moves outside in the radial direction. In order to obtain continuous and stable arc on magnetic materials and uniform erosion of the target, it is necessary to re-design the configuration of the cathode. The cathode configuration designed for deposition of magnetic materials is schematically shown in Fig. 1b. A cylinder made of a soft magnetic material such as pure Fe surrounds the magnetic target. A boron nitride (BN) ceramic ring was placed on top of the magnetic target. The design was mainly based on the following principles: when a BN ring is placed on a magnetic material, the arc spot moves randomly within the ring and the target erosion is uniform. The BN ring is used to confine the motion of arc spot within the ring. BN ceramic has a low surface energy for most metals and low emission efficiency of secondary electrons, which can prevent the arc spot from moving on the surface of the BN ring and reduce the deposition of the target material on the surface of the BN ring. Using this new cathode design, a stable and continuous arc can be J.S. Chen et al. / Thin Solid Films 443 (2003) 115–119 117 Fig. 3. The surface roughness of the FeNi films as a function of substrate bias. Fig. 2. AFM images of FeNi films deposited at (a) y100 V and (b) y400 V. function of bias conditions. The rms roughness decreases from floating condition (0 V) to y100 V, and then increases as the bias increases from y100 to y400 V. The XRD spectra of the films deposited at various biases are shown in Fig. 4a. For the sample prepared at floating condition, the FeNi(111) and (200) peaks are observed. When a bias of y100 V is applied, the intensity of FeNi(111) and (200) peaks increases. By further increasing the substrate bias, the intensity of obtained and the erosion pattern is uniform for magnetic target. 3. FeNi films deposition and properties In this work, permalloy Fe0.2Ni0.8 films were deposited on Si (100) substrate at room temperature using the new cathode design and the arc current was set to 100 A. The toroidal magnetic field was fixed at 40 mT. The substrate was negatively biased from y100 to y400 V with respect to the ground (anode). The deposition rate was approximately 0.1 nmys. The surface morphology and roughness of the films were examined using atomic force microscope (AFM, Digital Instruments) in tapping mode. The value of root-mean-square (rms) surface roughness was evaluated in the area of 2=2 mm. The crystallographic structure of films was determined by Rigaku grazing X-ray diffractometer (GXRD) with Cu ˚ at 50 kV and Ka1 excitation (wavelength of 1.5406 A) 20 mA. The angle between the incident X-ray and the surface of the films was fixed at 0.58 and the diffraction pattern was obtained by changing the position of the counter with a step of 0.058. Magnetic properties were measured at room temperature by Lakeshore vibrating sample magnetometer (VSM, Model 7300). The typical AFM images of the films deposited with the substrate bias of y100 and y400 V are shown in Fig. 2. All of the images show island-like features. Fig. 3 shows the root mean square (rms) roughness as a Fig. 4. (a) XRD spectra and (b) FWHM of peak (111) of FeNi films deposited at various substrate bias. 118 J.S. Chen et al. / Thin Solid Films 443 (2003) 115–119 FeNi(111) and (200) peaks decreases. Fig. 4b presents the variation of the full width at half maximum (FWHM) of peak (111) with the substrate biases. The FWHM as a function of the substrate bias has a trend similar to the roughness. With a bias of y100 V, the FWHM reaches its minimum, reflecting the optimal crystalline quality of the films. One of the most important factors affecting the morphology and structure of the films is the lateral mobility of the adatoms on the substrate. With a bias of y100 V, most of the ions energy is changed into the lateral energy after bombardment on the substrate and adatoms mobility increases. So the film at the bias of y100 V shows smoother morphology and better crystallinity than that of the sample under floating condition. Although lateral ion energy also increases with further increase of the bias, the ion energy along normal component is increased more, which causes the increase of the roughness. The magnetization–hysteresis (M–H) loops of FeNi films with various substrate biases are shown in Fig. 5. The films deposited at lower substrate bias (0 and y100 V) have the expected square M–H loops while the films deposited at higher substrate bias have poor M–H loops with two distinctive slopes before saturation. It has been recognized that the smaller slope before saturation is due to a perpendicular anisotropy component normal to the plane of the film w14–16x. The mechanisms for producing perpendicular anisotropy include the following: (1) magnetocrystalline anisotropy—if the FeNi films is (100) textured, the film’s normal is the easy axis in the absence of shape aniso- Fig. 6. The saturated magnetization 4pMS and coercivity Hc of the FeNi films as a function of substrate bias. tropy; (2) microshape anisotropy—the columnar structure of the magnetic grains separated by a non-magnetic phase or voids can produce a microshape anisotropy along the column axis; (3) magnetoelastic anisotropy— when the film is under a compressive stress, the magnetoelastic energy favors the magnetization orientated out of the plane of the film. Further investigation is currently under way to determine which kind of anisotropies play the dominant role. The saturated magnetization 4pMS and coercivity Hc as a function of substrate bias are shown in Fig. 6. When the bias is y100 V, the film shows the lowest coercivity and the largest saturated magnetization. The X-ray photoelectron spectroscopy (XPS) results (not shown) indicate that the composition of the films of permalloy, fcc-FexNi1yx, where x ranging from 0.19 to 0.21, is nearly independent on the substrate bias. Thus the changes in saturated magnetization and coercivity Fig. 5. M–H loops of FeNi films deposited at various substrate bias, (a) 0; (b) y100 V; (c) y200 V; (d) y400 V. J.S. Chen et al. / Thin Solid Films 443 (2003) 115–119 with bias are not induced by the slight variation of composition. The film with good soft magnetic properties has the lowest surface roughness and better crystallinity, which are consistent with Fe films deposited by dual ion beam sputtering w17x. 4. Conclusions In summary, magnetic Fe0.2Ni0.8 films have been successfully deposited on silicon substrate using the modified cathode design. A stable and continuous arc with uniform target erosion can be obtained. When the substrate bias is y100 V, the film exhibits the lowest coercivity and highest saturated magnetization among all the investigated conditions, which may be related to its good surface roughness and crystallinity. References w1x S. Iwatsubo, T. Takahashi, M. Naoe, J. Appl. Phys. 83 (1998) 6667. w2x T.T. Honda, K.I. Arai, M. Yamaguchi, J. Appl. Phys. 76 (1994) 6994. w3x J.C. Huang, Y.M. Hu, C.C. Yu, J. Appl. Phys. 83 (1998) 7046. 119 w4x W.D. Davis, H.C. Miller, J. Appl. Phys. 40 (1969) 2212. w5x H.C. Miller, J. Appl. Phys. 66 (1989) 1107. w6x I.I. Aksenov, S.I. Vakula, V.G. Padalka, V.E. Strel’nitskii, V.M. Khoroshikh, Sov. Phys. Tech. Phys. 25 (1980) 1164. w7x T.D. Schemmel, R.L. Cunningham, H. Randhawa, Thin Solid Films 181 (1989) 597. w8x P.J. Martin, R.P. Netterfield, T.J. Kinder, L. Descotes, Surf. Coat. Technol. 49 (1991) 239. w9x R.L. Boxman, S. Goldsmith, A.B. Shalom, L. Kaplan, D. Arbilly, E. Gidalevich, V. Zhitomirsky, A. Ishaya, M. Keidar, I. Beilis, IEEE Trans. Plasma Sci. 23 (1995) 939. w10x X.L. Xu, S.P. Lau, B.K. Tay, Thin Solid Films 398–399 (2001) 244. w11x P. Siemroth, T. Schulke, T. Witke, IEEE Trans. Plasma. Sci. 25 (1997) 571. w12x J.C. Sherman, R. Webster, J.E. Jenkins, R. Holmes, J. Phys. D: Appl. Phys. 8 (1975) 696. w13x E. Hantzsche, B. Juttner, IEEE Trans. Plasma Sci. 13 (1985) 230. w14x K. Sin, C-T. Wang, S.X. Wang, B.M. Clemens, J. Appl. Phys. 81 (1997) 4507. w15x B. Viala, M.K. Minor, J.A. Barnard, J. Appl. Phys. 80 (1996) 3941. w16x N. Satio, H. Fujiwara, Y. Sugita, J. Phys. Soc. Jpn. 19 (1964) 1117. w17x S. Iwatsubo, T. Takahashi, M. Naoe, Thin Solid Films 67 (1999) 343.