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Journal of The Electrochemical Society, 152 4 C190-C195 2005

0013-4651/2005/152 4 /C190/6/$7.00 The Electrochemical Society, Inc.

Pulse-Reverse Electrodeposited Nanograinsized CoNiP Thin Films and Microarrays for MEMS Actuators
Shan Guana,*,z and Bradley J. Nelsonb
a b

Department of Mechanical Engineering, University of Minnesota-Twin Cities, Minneapolis, Minnesota 55455, USA Institute of Robotics and Intelligent Systems, Swiss Federal Institute of Technology (ETH), Zurich, Switzerland

This paper reports on a low residual stress hard magnetic CoNiP alloy electrodeposition technique for microelectromechanical systems MEMS applications based on techniques previously developed for CoNiP thin lms for perpendicular magnetic recording. Besides electrolyte chemicals, various processing parameters including applied current density, lm thickness, electrolyte agitation, electrolyte pH, and temperature are optimized to provide thick lms with low residual stress. The resulting hard magnetic CoNiP alloy exhibits a relatively high perpendicular coercivity Hc of around 700-1200 Oe and a high saturation magnetization M s of 0.41-0.52 kG. Thick lms up to 52 m with a low residual stress have been realized using this CoNiP electrodeposition technique. In addition, CoNiP microarrays 22.5 m thick are surface micromachined for the integrations with magnetic MEMS devices. Experimental results conrm that these microarray congurations have a higher coercivity and maximum magnetic energy density, BH max, than thin lms in the perpendicular direction. 2005 The Electrochemical Society. DOI: 10.1149/1.1862476 All rights reserved. Manuscript submitted June 21, 2004; revised manuscript received September 21, 2004. Available electronically March 1, 2005.

Magnetic microelectromechanical systems MEMS actuators have the advantages of low power consumption, large displacement, and large actuation force. Unfortunately, it is difcult to integrate hard magnetic materials into MEMS fabrication because of incompatibilities between hard magnetic deposition techniques and many standard MEMS fabrications processes.1 Electrodeposition is a technique that is generally compatible with MEMS fabrication. Furthermore, it has fast deposition rates, does not require a vacuum system, is relatively low cost, and can deposit various materials.2,3 However, electrodeposition of hard magnetic lms suitable for MEMS actuators has not been successfully developed because achieving lms with appropriate material properties has proven difcult due to factors such as high residual stress and insufcient magnetic properties. Co-based alloys such as CoNiMnP or CoNiP exhibiting a perpendicular coercivity have been electrochemically deposited,4-9 for use as perpendicular magnetic recording media. Luborsky6 examined the effects of group VA e.g., P, As, Sb, and Bi and VIB e.g., W, Mo, and Cr as additives on the coercive force of electrodeposited Co-Ni lms. All these elements are capable of increasing the coercivity of Co-Ni lm to some degree. The most effective element is phosphorus P . However, the studied lm thickness is less than 1 m, and the maximum coercivity obtained is about 1020 Oe, which cannot satisfy typical MEMS applications. Osaka et al.10,11 investigated the potential applications of electroless deposited Co-Ni-Re-P for perpendicular recording media. The electroless plated Co-Ni-Re-P alloys have a perpendicular coercivity of about 440-1270 Oe and a saturation magnetization M s of 104-252 emu/cm3. However, the maximum thickness obtained is only about 0.5 m because it is difcult to deposit thick lm by electroless plating. In addition, the reported electroless plating technique requires a relatively high temperature of 80C and a basic electrolyte pH 9.2 ;11 thus, it is not suitable for plating though the photoresist mask using this technique. Horkans et al. investigated the magnetic properties of electrodeposited CoNiMnP alloys with a magnetic anisotropy normal to the substrate.4 The M-H hysteresis loops show that a thin lm 100 nm thick has an Hc around 1515 Oe and an M r of about 6.71 104 emu. The thickness of the lms affected the magnetic properties, and to obtain an anisotropic vertical Hc a minimum thickness of 50 nm is needed.4 Liakopoulos et al. applied Horkans technique to electrodeposit magnetic arrays of CoNiMnP alloys containing 1500 40 40 50 m magnets in a cube-like shape on a 2.5 2.5 mm silicon

substrate.12 Hysteresis loops show that the CoNiMnP arrays have a vertical coercivity around 380-500 Oe and a residual induction Br of about 0.5-0.8 kG. These magnetic properties can be improved greatly with the addition of an external magnetic eld during the electrodeposition. The reported CoNiMnP microarrays fabricated in the presence of an external magnetic eld have a coercivity of 710-1100 Oe.9 However, the addition of electromagnets during electrodeposition increases the complexity of the system. Myung et al.7,8 examined the effect of electrolyte pH on the crystal structure of CoNiP deposits. They found that a low pH promotes the facecentered cubic phase and a high pH promotes the hexagonal closepacked phase of cobalt. CoNiP hard magnetic materials electrodeposited from their reported electrolytes reach a maximum perpendicular coercivity of about 750 Oe at an electrolyte pH of 2.5. The coercivity remains constant in the pH range of 2.5-6.0. An electrochemically deposited Co-based alloy such as electrodeposited CoNiP is a desirable magnetic material for MEMS actuators because of its relatively high coercivity and BH max. However, because magnetic force depends on material volume, it is often necessary to electrodeposit thick lms more than 10 m for MEMS. In this case, the residual stress induced by electrodeposition becomes a dominant factor governing device yield. Unfortunately, there are no detailed investigations on controlling residual stress in electrodeposited CoNiP lms. In addition, existing CoNiP electrodeposition techniques are not suitable for thick lm deposition because magnetic properties, especially coercivity, appear to decrease rapidly with an increase in lm thickness.7 Generally, cobaltbased hard magnetic thin lms electrodeposited from an aqueous electrolyte have relatively high tensile residual stress, especially those lms with a relatively large thickness 10 m .13 Our experimental results show that residual stress in the electrodeposited CoNiMnP thin lms using Horkans reported technique4 is high and can result in lm microcracks see Fig. 1, for example . A comprehensive study on the effects of various parameters on residual stress is greatly needed, and a technique that can deposit CoNiP lms with lower residual stress as well as relatively good magnetic properties is extremely useful for MEMS. This paper investigates several factors inuencing residual stress in CoNiP electrodeposition and describes an optimized CoNiP electrodeposition technique capable of fabricating microarray structures for magnetic MEMS actuators. Experimental Electrodeposition of CoNiP.The CoNiP thin lms are electrodeposited on 4 in. silicon wafers using the optimized electrolyte listed in Table I. The silicon substrates are rst immersed in an

* Electrochemical Society Active Member.

z

E-mail: shan.guan@kodakversamark.com

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Figure 1. SEM image of CoNiMnP electroplated lm deposited using Horkans technique lm thickness 5 m .

H2SO4 + H2O2 bath heated to 120C for 30 min followed by immersion in 10:1 buffered oxide etch buffered HF to remove organics. A 2000 Si3N4 insulating layer is deposited using low pressure chemical vapor deposition and then sputtered with a plating seed layer of Cr 400-500 /Au 1500-2500 at a chamber base vacuum of 1 106 Torr. Electrodeposition processing is controlled using a Dynatronix pulse reverse power supply. The total forward current for deposition is set to be twice that of the reverse current for dissolution of the deposits. The pulse electrodeposition current Ia can be expressed as Ia = td td + tp Ip 1

Figure 2. Process ow of microarray fabrication.

Characterization.The electrodeposited lm thickness is measured by a DekTak prolometer. Wafer curvatures before and after electrodeposition are measured by an ADE microsense 314A-385 wafer bow, and the residual stress of the electrodeposited lms is calculated according to the Stoney equation14
f

2 E sd s 1 6R 1 s df

where td and tp denote the pulse duration and pause, respectively. Ip is the pulse current. In the CoNiP thin lm and microarrays deposition, td equals tp, so the pulse electrodeposition current Ia equals half of the pulse current Ip. Fabrication of CoNiP microarray magnets.The microarrays are fabricated using the process shown in Fig. 2. The general fabrication procedure for microarray magnets is described as follows. Step a. RCA-clean a blank 100 p-type silicon wafer to remove all organics and oxides from the surface. Then oxidize wafer with 5000 of SiO2. Step b. Sputter an adhesion layer of 500 chromium and an electrical conduction layer of 1500-2000 gold. Step c. Spin on AZ-9260 positive photoresist. Pattern the photoresist to form electrodeposition molds. Step d. Pulse reverse electrodeposit CoNiP microarray magnets with moderate electrolyte agitation. Step e. Remove photoresist with acetone. Step f. Wet etch plating seed layers of Cr and Au.

where f denotes the lm residual stress; ds and df denote the thickness of substrate ds = 506.3 m for silicon wafers with plating seed layers and lm, respectively; R is the radius of curvature of the wafer with an electrodeposited lm, and Es and s are Youngs modulus and Poissons ratio of the silicon substrate, respectively. The electrodeposited CoNiP surface morphology is examined by scanning electron microscopy SEM . The surface roughness of these lms is measured by a prolometer, and the three-dimensional 3D scanning image is created based on a scanning area of 500 500 m. The magnetic properties of the CoNiP are determined by M-H loops measured at room temperature with a sample area of 0.5 0.5 cm using a vibrating sample magnetometer VSM . These M-H loops are transformed into B-H loops to provide information on the residual induction Br. In addition, the maximum energy density, BH max, of electrodeposited permanent magnets is calculated by using data chosen from the points on the second quadrant branch of the B-H loop that give the largest area for an enclosed rectangle.15 Results and Discussion Residual stress in electrodeposited CoNiP thin lms.The electrolyte composition listed in Table I is experimentally optimized to provide lms with the minimum electrodeposition-induced residual stress. Nickel-sulfamate Ni- NH2SO3 2 and cobalt-sulfate CoSO46H2O are used for the metal ions source for Reactions 3 and 4. The voltages are expressed vs. saturated calomel electrode SCE Co2+ + 2e Co E0 = 0.75 V vs. SCE Ni2+ + 2e Ni E0 = 0.50 V vs. SCE 3 4

Table I. CoNiP electrodeposition electrolyte composition. Plating bath composition g/L CoSO46H2O Ni NH2SO3 24H2O Na2SO4 HBO3 NaH2PO22H2O Sodium saccharin 30-35 28-30 20-25 30-45 6.0-7.0 0.75-1.0

Na2SO4 can increase the conductivity of the electrolyte, without itself being involved in the electrode electrochemical reactions. HBO3 has a similar function in increasing electrolyte conductivity,

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Figure 3. Effect of sodium saccharin concentration on lm residual stress.

Figure 5. Effect of CoNiP lm thickness on residual stress.

and it also acts as a pH buffer agent to keep the electrolyte pH stable, which is extremely important because the coercive eld of electrodeposited CoNiP alloys is strongly dependent on the electrolyte pH.4,7 NaH2PO22H2O supplies the ions for the reactions H2PO + 2H+ + e P + 2H2O E0 = 0.50 V vs. SCE 2 on the cathode and H2PO 2 + H 2O H2PO 3 + 2H + 2e
+

applied in chromium, nickel, and magnetic materials electroplating.19,20 It can reduce or even eliminate the concentration polarization and, thus, enhance the activation polarization, activation. The critical radius of the surface nucleus Rc is inversely proportional to
3 activation

Rc = E0 = 0.75 V vs. SCE 6

s ze
activation

on the anode. Sodium saccharin is used as the residual stress reliever in the electrolyte. Figure 3 indicates that sodium saccharin can effectively reduce residual stress when its concentration in the electrolyte exceeds 0.75 g/L. The electrodeposition process is controlled using a pulse-reverse current source. The reversed current technique is commonly used in electrodeposition, especially in the electroforming of thick lms lm thicknesses are sometimes greater than 2000-5000 m . When a reversed current is applied in the cathodic duration the electrodeposition takes place, while in the anodic duration the deposited lm is electrochemically etched. Consequently, smooth lms with low residual stress can be obtained.16-18 Current pulsing has been

where s is the area occupied by one atom on the surface of the nucleus; is the edge energy; z denotes the transference electron numbers in a certain electrode reaction, and e equals 1.062 1019 C. As seen from Eq. 7, materials deposited using pulse current tend to have a smaller grain size. Various processing factors such as current density and electrolyte agitation also inuence lm residual stress, and it is necessary to understand their effects on residual stress in a CoNiP electrodeposition process. The processing parameters involved in a CoNiP electrodeposition process can be divided into major and minor factors according to their inuence on residual stress. The major factors include lm thickness, applied current density, and electrolyte agitation; minor factors are electrolyte pH and temperature. To investigate the effects of different processing parameters on residual stress, the electrolyte listed in Table I is used. The contributions of major processing parameters to the residual stress in a CoNiP electrodeposition process decrease in a sequence of applied current density, lm thickness, and agitation technique. The most important factor affecting lm residual stress is applied current density. As seen from Fig. 4. The lm residual stress increases rapidly with an increase in current density when the lm thickness is xed. When the current density reaches 10 mA/cm2, the lm tensile residual stress is about 7.8 MPa. As the current density increases to 20 mA/cm2, the lm tensile residual stress is as high as 11.4 MPa, an increase of about 50%. In the measured current density range of 0.5-25 mA/cm2, the corresponding lm residual stress can be approximated by

Table II. Effect of electrolyte agitation on lm residual stress. Film thickness is 10 m. Agitation method None Mechanical Nitrogen Mechanical Tensile residual stress MPa 8.6 7.0 6.8 6.9

Figure 4. Effect of current density on residual stress of the lm investigated lm thickness 10 m .

nitrogen

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Table III. CoNiP hard magnetic material electrodeposition processing parameters.

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Electrolyte composition Power source Anode Applied current density Electrolyte pH Electrolyte temperature Electrolyte agitation

Refer to Table I for details. A pulse-reverse power supply Insoluble platinum-titanium Pt-Ti alloys 1-20 mA/cm2 2.0-4.5 25-45C Nitrogen agitation

= k 1I 2 + k 2I + k 3

8
Figure 7. 3D surface roughness prole of pulse-reverse electrodeposited CoNiP hard magnetic thin lm 15 m thick.

where denotes lm tensile residual stress, I denotes applied current density, and kn are constants varying with the lm thickness. For example, when the lm thickness is about 10 m, the residual stress can be represented by = 0.00881I2 + 0.54934I + 3.54953 9 This relationship can be used to predict residual stress affected by applied current density for a given lm thickness in CoNiP electrodeposition. As the magnetic force generated by permanent magnets is proportional to the volume of magnetic materials, the investigated lms are thicker than 4 m. Figure 5 demonstrates the effect of lm thickness on residual stress. At a low applied current density of 1 mA/cm2, the tensile residual stress in the CoNiP stabilizes after the lm thickness exceeds 15 m. However, at a higher current density such as 15 mA/cm2, the residual stress remains stable after the lm thickness exceeds 10 m. This phenomenon agrees with what has been observed from nickel electrodeposition processes.21 Experimental results show that another important factor affecting residual stress is electrolyte agitation. There are many reports on reducing lm residual stress by various electrolyte agitation techniques.22,23 By agitating the electrolyte during electrodeposition, the concentration polarization within the double layer area is reduced. This can promote a more even distribution of real current density across the wafer surface, giving a smooth coating surface, decreasing the number of surface defects, and thus reducing the residual stress induced by electrodeposition. The effects of agitation on residual stress in the CoNiP electrodeposition process are listed in Table II for a lm thickness of 10 m. As revealed in Table II, electrolyte agitation using both nitrogen and mechanical stirring can effectively reduce residual stress. However, there is no obvious improvement with a combination of the two techniques. Compared with current density, lm thickness, and electrolyte agitation, the inuence of electrolyte pH and temperature on lm residual stress is much smaller. Therefore, a low residual stress CoNiP lm can be obtained by carefully regulating the major residual stress inuence factors.

Pulse-reverse electrodeposited CoNiP thin lms.Based on the experimental results obtained in the last section; an optimized CoNiP hard magnetic alloy electrodeposition technique is developed, and the electrolyte and process parameters are listed in Table III. The CoNiP lm electrodeposited using this technique has extremely low residual stress. For example, the CoNiP thin lm deposited on a silicon wafer has a tensile stress of about 2.9 MPa at a thickness of 52 m, which compares very well with that of nickel obtained in a nickel sulfamate bath.21 Figure 6 shows SEM images of the surface micromorphology of the pulse-reverse electrodeposited CoNiP with a thickness of 15 m using different current densities. In both cases, the CoNiP alloy has a nanoscale grain size, while materials deposited using a higher current density of 12 mA/cm2 have a smaller grain size approximately 50-60 nm than materials deposited using a lower current density of 2 mA/cm2 approximately 200-250 nm . The surface roughness of the CoNiP lm is measured by a prolometer, and a 3D scanning image is shown in Fig. 7. The CoNiP lms have a relatively smooth surface with a root-mean-square deviation roughness of 120.1 and an arithmetic mean deviation roughness of 55 . These measurement results conrm that the CoNiP lms deposited from the optimized electrodeposition technique are desirable for MEMS. Magnetic properties of CoNiP thin lms and microarrays.The pulse-reverse electrodeposited CoNiP alloy is a typical hard magnetic material in both the parallel and perpendicular directions to the substrate. However, it has a perpendicular anisotropy, i.e., the Hc in the perpendicular direction is 200-300 Oe larger than the Hc parallel

Figure 6. SEM images of CoNiP thin lms electrodeposited using current densities of left 2 mA/cm2 and right 12 mA/cm2. Investigated lm thickness is 15 m.

Figure 8. Effects of lm thickness on perpendicular coercivity of CoNiP alloy. Applied current 10 mA/cm2; pH and temperature of electrolyte are 4.0 and 30C, respectively.

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Table IV. Comparison of perpendicular magnetic properties of electrodeposited CoNiP thin lms and microarrays.

Materials CoNiP thin lm CoNiP microarrays

Hc kOe 0.7-1.2 0.8-1.3

Br kG 0.62-1.0 0.71-1.1

BH

3 max kJ/m 1.3-1.8 1.7-2.0

the direction normal to the lm plane.11 When a ferromagnetic material is magnetized, magnetic poles are created on the surface. These poles establish a demagnetizing eld Hd antiparallel to the magnetization M :15 Hd = NM 10 where N is the demagnetizing factor, which depends on the shape of the magnets. The generated magnetic eld of a permanent magnet must be adjusted by this demagnetizing eld
Figure 9. SEM images of micromachined CoNiP microarrays.

H = Happlied NM

11

to the wafer substrate. This is in agreement with other reports on coercivity of electrodeposited CoNiP hard magnetic materials.4-12 In the perpendicular direction, the CoNiP has a coercivity of about 700-1200 Oe and an M s of 0.41-0.52 kG. The M s of the CoNiP alloy is higher than that of the CoNiMnP M s = 0.36-0.50 kG due to the absence of the antiferromagnetic element of Mn.24 Experimental results reveal that perpendicular coercivity of CoNiP is insensitive to lm thickness after it exceeds approximately 10 m, as shown in Fig. 8. The CoNiP lm retains a relatively high and stable perpendicular coercivity of about 850 Oe when the thickness is greater than 10 m, which demonstrates that the optimized CoNiP electrodeposition technique is suitable for depositing thick lms for MEMS actuators. The structure of microarrays is useful in integration of electrodeposited hard magnetic materials with silicon-based MEMS devices because of the suppression of the residual stress between magnets and the silicon substrate.9,25 CoNiP microarrays are fabricated using the process demonstrated in Fig. 2. Figure 9 shows SEM images of CoNiP arrays of dimensions 50 30 22.5 m L W H for a single element. Ahn et al.9,12 believe that their electrodeposited CoNiMnP microarrays with a structure similar to that of the CoNiP arrays we obtained can be approximated as a sphere with a demagnetizing factor of 1/3 in the perpendicular direction, while it is generally believed that thin lms have a demagnetizing factor of 1 in

Therefore, the CoNiP microarray structure has a higher generated magnetic eld compared to the CoNiP thin lm deposited under the same conditions. The magnetic properties of the CoNiP arrays are determined using a VSM. Figure 10 demonstrates both the typical M-H loops of CoNiP microarrays and thin lms 22.5 m thick for the perpendicular direction for comparison. Table IV lists the details of the perpendicular magnetic properties of CoNiP microarrays and thin lms. Experimental results show that compared with thin lms, the CoNiP microarrays have a higher coercivity, residual induction, and maximum magnetic energy density. Thus, they are well suited for use as magnetic MEMS actuator components in the perpendicular direction to the substrate. Conclusions A CoNiP hard magnetic alloy electrodeposition technique that provides thick lms more than 10 m with extremely low residual stress is described. The technique is particularly well suited for magnetic MEMS actuator components. The effects of both electrolyte composition and processing parameters on the residual stress of CoNiP thin lm are investigated. The pulse-reverse electrodeposited CoNiP lms exhibit a low surface roughness as well as a relatively high perpendicular coercivity. CoNiP microarrays are fabricated to lower the residual stress for integration with magnetic MEMS actuators. Magnetic property measurements show that magnetic properties such as BH max have been improved, which indicates that microarrays are appropriate structures for magnetic MEMS actuators. Acknowledgments The authors thank Seagate Technologies for partially supporting this research. We also thank the Institute for Rock Magnetism at the University of Minnesota for the use of their magnetic properties testing facilities.
The Swiss Federal Institute of Technology assisted in meeting the publication costs of this article.

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Figure 10. M-H loops of CoNiP thin lms and microarrays in the perpendicular direction to the substrate.

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8. 9. 10. 11. 12. 13. 14.