M. MA^EK, A. OBLAK: Ni-Fe ALLOY THIN FILMS FOR AMR SENSORS 499–501 Ni-Fe ALLOY THIN FILMS FOR AMR SENSORS TANKE PLASTI ZLITINE Ni–Fe ZA IZDELAVO AMR-SENZORJEV Marijan Ma~ek1, Alen Oblak2 1University of Ljubljana, Faculty of Electrical Engineering, Tr`a{ka 25, 1000 Ljubljana, Slovenia 2LEK, Verov{kova 57, 1000 Ljubljana, Slovenia marijan.macek@fe.uni-lj.si Prejem rokopisa – received: 2016-07-15; sprejem za objavo – accepted for publication: 2016-09-19 doi:10.17222/mit.2016.203 Ni-Fe alloy films deposited in sputtering apparatus and the subsequent AMR sensor fabrication were successfully developed. The results on test devices are comparable to the commercially available device with AMR as measured on the standard multipole magnetic tape. Keywords: Ni-Fe alloy, AMR, sputtering Razvit je bil postopek napr{evanja in kasnej{e obdelave tankih plasti zlitine Ni-Fe, potrebnih za izdelavo senzorjev AMR. Rezultati testnih uporov, merjenih na standardnem, mnogopolnem magnetnem traku, so primerljivi s komercialnimi senzorji. Klju~ne besede: zlitina Ni-Fe, AMR, napr{evanje 1 INTRODUCTION Magnetoresistance (MR) is a phenomenon that reflects the effect of an external magnetic field on the resistance change of certain materials. Among known MR the anisotropic magnetoresistance phenomenon (AMR) is widely used in the field of position sensors and encoders due to its robustness compared to optical ones. The AMR effect arises from spin–orbital coupling and therefore depends on the angle  between the magnetic moment M and the current j.1 Therefore, resistivity  is a function of  and can be written as in Equation (1), where the symbols  and I denote the perpendicular and parallel components:     = + ⊥sin cos2 2 (1) The response, i.e., the difference between both com- ponents of resistivity, of AMR sensors strongly depends on the soft ferromagnetic material properties. A very common choice are NixFe1–x alloys, known under commercial name Ni–Fe alloy with typical concentration x close to 0.8. The properties of thin layers however de- pend on the deposition parameters (pressure, tempera- ture, deposition rate, applied magnetic field), subsequent annealing and of course on the layer thickness. Conditions should be set in such a way as to obtain a highly oriented crystalline structure. In the absence of an external field during the film’s deposition the correct deposition condition leads usually to the (111) preferred orientation of film with the easy axis of magnetisation perpendicular to the surface. For other orientations of the easy axis, an external magnetic field of 5–15 kA/m during deposition or subsequent annealing is essential. In our work we concentrate the efforts in order to sputter deposit thin films of Ni–Fe from a Ni80Fe20 target without an external magnetic field. Therefore, we are limited in variation of deposition parameters (power P and Ar pressure pAr), which influence the deposition rate and the chemical constitution1 of the deposited films and on to the effects of subsequent annealing at temperatures from 150 °C to above 400 °C in forming gas (10 % H2 in N2). 2 EXPERIMENTAL PART Thin Ni–Fe films were deposited onto 500-nm-thick thermally grown SiO2 on 100-mm Si test wafers. The depositions were performed in Perkin Elmer Sputtering Model 2400 apparatus working at a base pressure below 1.3×10–4 Pa from a Ni80Fe20 target. The pressure of the Ar during the sputtering was set to 1.1 Pa as first results suggest that higher pressures give unsatisfactory results. The Ni–Fe alloy films were usually deposited onto a buffer layer in order to promote preferential (111) crystallite orientation. A very common buffer is Ta, but (Ni0.81Fe0.19)0.66Cr0.34 layer2 gives better results. We tried to simulate the NiFeCr depositing thin layer of Cr/NiFe/Cr in the way to reach preferred ratio between Cr and Ni–Fe alloy. The resistors were defined by the so-called lift-off process since with standard positive PR process and subsequent etching in Ni etchant the minimum dimen- sion could not be kept in the desired limits. For test resistors devices with two different geometries LxW (500×25 μm2, 150×3 μm2) from the laboratory test vehicles. After the finished "lift-off" step test and device MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Materiali in tehnologije / Materials and technology 51 (2017) 3, 499–501 499 UDK 669.24:669.15:621.793 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 51(3)499(2017) wafers were annealed in quartz tube in forming gas (10 % H2 in N2) atmosphere at different temperatures 200–420 °C. The device wafers were finished by the standard double metal process with the highest tempera- ture 350 °C during inter-metal dielectric deposition. The properties of the AMR layers were analyzed on test samples by XRD analysis and magnetic measure- ments by a Lake Shore 7307 vibrating-sample magneto- meter. On the same test wafers sheet resistance and surface roughness were measured after different anneal- ing steps. The sheet resistance was measured by a 4–point probe and roughness by a laser scanning micro- scope. The AMR measurements of the resistors were made in a measured magnetic field of permanent magnet or multipole magnetic tape with periodic magnetization as used for standard applications with 2 = 4 mm. The results on the tape were also compared to the results of single resistor from commercial AMR encoder bridge structure. 3 RESULTS AND DISCUSSION The AMR effect is inversely proportional to the thickness, but unfortunately the coercivity Hc limits the lower thickness to about 50 nm.1 The layer thickness t can be calculated from the measured sheet resistance Rsh and the known resistivity , t = /Rsh. Unfortunately, in thin films the resistivity depends on its thickness and structure as modeled by 3. The accepted values are 123±30 nm,4 but H. Faltin5 observed even 196 nm for 120-nm-thick films deposited onto Si. Not at least, within the fixed geometry the resistivity of single resistor of about 1 k is the optimum one. Therefore, an opti- mum Rsh is between 5 /sq and 10 /sq. To characterize the AMR films their sheet resistance Rsh was measured after different processing steps, and after isochronal (30 min) annealing in forming gas. The results are shown in Figure 1. There is a rapid change in Rsh for the samples deposited without a buffer layer. The layers deposited onto the buffer exhibit a moderate reduction in the resistivity up to the annealing at 350 °C, which is also the highest temperature in the process. Generally speaking, samples without buffer, and samples deposited with lower power have a higher Rsh. Since the sputtering energy P.t was set to 17 kJ the difference is in the layer structure. The final Rsh was 8–12 /sq, close to our demands for an AMR sensor. Annealing at 400 °C and 420 °C does not significantly change the resistance, but microscopic investigations show unwanted changes in the structure of the film and an increase in the surface roughness Sra from 10–20 nm to over 50 nm, especially for films deposited without a buffer. The reduction of Rsh after annealing at 350 °C indicates strong changes in the crystal structure of the Ni–Fe alloy layer. The XRD analysis in Figure 2 shows changes in the preferred (111) orientation after annealing up to 350 °C. Annealing at higher temperatures has no effect on the orientation of the crystallites. In the XRD pattern a weak (200) Cr peak is also observed as well a strong (400) Si. Obviously our presumption for buffer layers does not work. In any case, the Cr buffer has some beneficial effects on the surface roughness and it signifi- cantly reduces the sheet resistivity of at least the annealed samples. The magnetic properties of the deposited AMR layers are shown in next Figure 3. From rather rough plot we can see a distinctive difference between the plots for easy axis of magnetization (full circles), perpendicular orientation of magnetic field to the surface and hard axis (open circles), lying parallel to the surface. From this plot the coercivity Hc is estimated to be 5kA/m. Since these are the very first experiments, the effects of pro- M. MA^EK, A. OBLAK: Ni-Fe ALLOY THIN FILMS FOR AMR SENSORS 500 Materiali in tehnologije / Materials and technology 51 (2017) 3, 499–501 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 2: XRD pattern for a layer deposited onto buffer layer at 400 W and pressure 1.1 Pa after deposition and isochronal annealing at (250, 350 and 420) °C Slika 2: XRD-vzorec plasti, nanesene pri 400 W in tlaku 1.1 Pa na vmesno plast po nanosu in izokronalnih popu{~anjih na (250, 350 in 420) °C Figure 1: Rsh measured after the deposition and isochronal annealing in forming gas; crosses denote sheet resistances for films deposited without buffer layer Slika 1: Plastna upornost Rpl po nanosu in izokronalnih popu{~anjih v tvornem plinu; kri`i predstavljajo plastne upornosti filmov, nanesenih brez vmesne plasti cessing parameters on to magnetic properties and the structure revealed by XRD of soft ferromagnetic layers have not been studied yet. The first experimental AMR resistors show promis- ing results. In Figure 4 the responses R/Ravg of the two test resistors LxW = 500×25 μm with slight differences in the processing (W#10 without buffer, W#08 with buffer layer) and a commercial AMR encoder are shown. The measurements were performed on a commercially avail- able multipole magnetic tape with 2 = 4 mm in steps of 0.1 mm and at a distance of 1.5 mm above the tape with a manual manipulator in all cases. From Figure 4 it is clear that there is no significant difference between both test samples, but their responses (~1.7 %) are somewhat lower than that on the commercial (~1.9 %) sensors. 4 CONCLUSIONS The first AMR resistors were successfully fabricated by sputtering of Ni–Fe alloy Ni80Fe20 in a Perkin Elmer apparatus and the necessary process steps for the subsequent annealing and fabrication of the resistors with predefined geometries with minimum dimensions W = 3 μm were established. The results from tests of the AMR resistors were comparable to the commercial one and encourages us to proceed with the development of extrapolators of custom design. Acknowledment The authors acknowledge RLS company and especially director Mr. J. Novak and their employees Mrs. D. Domanjko and Mr. M. Jane`i~ for support and encouraging during the first steps of AMR material process research and work on the design of the test encoder. Authors acknowledge dr. S. Gyergyek and dr. M. Spreitzer of the Jozef Stefan Institut, Ljubljana, for magnetic properties and XRD measurements. 5 REFERENCES 1 A. V. Svalov, R. Aseguinolaza, A. Garcia-Arribas, I. Orue, J. M. Barandiaran, J. Alonso, M. L. Fernández-Gubieda, G. V. Kurlyand- skaya, Structure and Magnetic Properties of Thin Ni–Fe alloy Films Near the Transcritical State, IEEE Trans Magn, 46 (2010) 2, 333–336 2 W. Y. Lee, M. F. Toney, D. Mauri, P. Tameerug, E. Allen, High Mag- netoresistance Permalloy Films Trough Growth on Seed layers of (Ni0.81Fe0.19)1–xCrx, IEEE Trans. Magn., 36 (2000) 1, 381–387 3 P. Wismann, K. Muller, Surface Physics, Springer-Verlag, Berlin 1975 4 A. C. Reilly, W. Park, R. Slater, B. Ouaglal, R. Loloee, W. P. Pratt Jr., J. Bass, Perpendicular Giant magnetoresistance of Co91Fe9/Cu Exchange-Biased Spin-Valves: A Further Test of the Unified Picture, JMMM, 195 (1999), L269–L274 5 H. A. Faltin, The Magnetic and Electrical Properties of Ni–Fe alloy- Carbon Thin Film Multilayers, thesis College of William and Mary, Virginia, USA 2000 M. MA^EK, A. OBLAK: Ni-Fe ALLOY THIN FILMS FOR AMR SENSORS Materiali in tehnologije / Materials and technology 51 (2017) 3, 499–501 501 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 4: A typical response R/Ravg of 2 test resistors and commer- cial reference to position over periodic multipole magnetic field with 2 = 4 mm at a distance of 1.5 mm Slika 4: Tipi~na krivulja odziva R/Ravg 2 testnih uporov in komer- cialne reference na pomik nad periodi~no spreminjajo~im magnetnim Figure 3: Magnetization curve for sample deposited with 400 W at 1.1 Pa, directly onto thermally grown SiO2 and annealed at 420 °C for 30 min Slika 3: Krivulja magnetizacije za vzorec nanesen pri 400 W in tlaku 1.1 Pa, direktno na termi~en SiO2 in popu{~ano 30 min na 420 °C