Diffusion analyses of non-ferromagnetic element in the cap-layer of post-annealed CoCrPt perpendicular media 著者 journal or publication title volume number page range year URL 齊藤 伸 IEEE transactions on magnetics 41 10 3187-3189 2005 http://hdl.handle.net/10097/35360 doi: 10.1109/TMAG.2005.855286 IEEE TRANSACTIONS ON MAGNETICS, VOL. 41, NO. 10, OCTOBER 2005 3187 Diffusion Analyses of Non-Ferromagnetic Element in the Cap-Layer of Post-Annealed CoCrPt Perpendicular Media Norikazu Itagaki1 , Shin Saito1 , and Migaku Takahashi1;2 , Member, IEEE Department of Electronic Engineering, Graduate School of Engineering, Tohoku University, Sendai 980-8579, Japan New Industry Creation Hatchery Center, Tohoku University, Sendai 980-8579, Japan This paper reports on the factors that dominate diffusion phenomena in post-annealed CoCrPt media with various cap-layer elements X. Hf- and Zr-capped media were found to show low diffusion temperature and have thin reacted layer in this experiments. These results are explained with following relationships revealed by detailed analyses of boundary diffusion and interdiffusion: 1) X with high melting point in cap-layer hardly starts boundary diffusion and interdiffusion, 2) X-capped media with higher melting point of CoX compound forms thinner reacted layer, and 3) X with low enthalpy of Co-X formation lead to low diffusion temperature. Index Terms—Hafnium, perpendicular magnetic recording media, post-annealing, zirconium. I. INTRODUCTION OR CoCr-based perpendicular media, to achieve both thermal stability and low intergranular exchange coupling is indispensable [1]. To solve this problem, several attempts, especially post-annealing, have been made focusing on the diffusion of non-ferromagnetic element from under- or cap-layer into the grain boundaries [2], [3]. We have already reported that remarkable exchange decoupling among magnetic grains was realized in the case of 410 C post-annealed media with Ti under- and cap-layers [4], [5]. This decoupling originates from not only boundary diffusion of Ti but also Co-Ti cohesions in grain boundaries. However, post-annealing causes interdiffusion, which leads to non-ferromagnetic reacted layer of CoTi phase with the B2 typed structure. The reacted layer brings magnetic spacing loss in recording. Furthermore, high post-annealing temperature is undesirable from a view point of mass production. In this paper, in order to reduce thickness of the reacted layer and the post-annealing temperature for post-annealed media, we investigated non-ferromagnetic material X, superior to Ti based on the detailed analyses of boundary diffusion and interdiffusion. TABLE I PROPERTIES OF CAP-LAYER MATERIALS X F II. EXPERIMENTAL PROCEDURE All the media were fabricated by the dc magnetron sputtering method in the ultraclean process [6]. The stacking structure of nm]/Ru the media was C[6 nm]/X[5 nm]/Co Cr Pt [ [5 nm]/Ti[25 nm]/crystallized glass disk substrate. Here, the were varied from 5 to nominal thickness of CoCrPt layer 30 nm. Ru underlayer was utilized on the purpose of both epitaxial growth of magnetic layer [7] and suppression of formation of reacted layer at the bottom of CoCrPt layer. Note that Ru has low reactivity with Co, Cr Pt, and Ti. The cap-layer materials X were Al, Hf, Nb, Ta, Ti, and Zr, which are insoluble in Co. , and dominant factors over chemical Melting point of Digital Object Identifier 10.1109/TMAG.2005.855286 coupling between Co and X, such as melting point of CoX compound, , and enthalpy of formation of Co-X interatomic are summarized in Table I. cohesion, The disks were heated by an infrared lamp run by constant power without exposure to the atmosphere. The substrate heating was performed up to 350 C for 13 s just after the deposition of the Ti under-layer. The post-annealing was carried out up to 160–420 C for 2–13 s just after the deposition of the cap-layer. The heating time is sufficiently short to suit the mass production. For structural analysis, X-ray diffraction profiles were obtained by grazing incident angle method (in-plane XRD; scan) using Cu-K radiation. The incident angle was 0.4 , which corresponds to about 20-nm-thick penetration of X-ray from the incident surface. The coercivities and saturation magnetizations were evaluated by vibrating sample magnetometer (VSM). III. RESULTS AND DISCUSSION A. Post-Annealing Effects for the Media With Various Cap-Layer Materials Fig. 1 shows coercivity normalized with that of media without post-annealing as a function of post-annealing temperature . Here, the value of slightly changes in the 0018-9464/$20.00 © 2005 IEEE Authorized licensed use limited to: TOHOKU UNIVERSITY. Downloaded on October 28, 2008 at 01:49 from IEEE Xplore. Restrictions apply. 3188 IEEE TRANSACTIONS ON MAGNETICS, VOL. 41, NO. 10, OCTOBER 2005 Fig. 1. Coercivity normalized with that of media without post-annealing as a function of post-annealing temperature for the media with X cap-layer. d of all the media is 20 nm. range of 4.5–5.1 kOe, depending on X. For the media without . On the cap-layer, over 250 C post-annealing degenerates other hand, for the media with any cap-layer materials, value clearly increases by post-annealing of adequate temperature. On the definition of diffusion temperature as the one at which value gains 5%, the Al-, Nb- and Ta-capped media show higher diffusion temperature of 370, 390, and 390 C than that of 360 C for the Ti-capped medium. In contrast, the Hf- and Zr-capped media show lower diffusion temperature of 240 or 280 C. The distinction of exchange decoupling among caplayer materials must be due to the different potential barrier to diffuse. Fig. 2 shows in-plane XRD profiles for the X-capped media post-annealed up to 420 C. The Nb- and Ta-capped media have diffracted lines from single phase of Nb and Ta. In cap-layer , the chemical coupling of each atom is material with high so strong and stable that interdiffusion hardly proceeds by annealing up to 420 C. On the other hand, the profiles of the Zr-, Hf-, Al-, and Ti-capped media show the diffracted lines from CoX reacted layers of the B2 typed structure. This suggests that interdiffusion occurs around X/CoCrPt interface in the same way as Ti-capped media [4]. Fig. 2. In-plane XRD profiles for the media with X cap-layer post-annealed to 420 C. The histogram below corresponds to powder pattern of hcp Co Cr Pt . Fig. 3. Schematic views of diffusion phenomena in the media (a) before and (b) after post-annealing. the X/CoCrPt interface. As a result, boundaries become non-ferromagnetic, and CoX reacted layer is formed. Taking account of the structural change mentioned above, we can simply derive the and averaged thickness of reacted layer in magnetic layer saturation magnetization of magnetic layer . These terms have a relation like the following equation: (1) B. Quantitative Evaluations for Boundary Diffusion and Interdiffusion Phenomena Next, we tried quantitative evaluations of boundary diffusion and interdiffusion separately through analysis of saturation magnetization. Fig. 3 shows a schematic view of diffusion phenomena in the post-annealed media. Light and dark gray circles represent CoCrPt and X atoms, respectively. Before post-annealing, the CoCrPt layer has hcp ferromagnetic grains surrounded by amorphous Cr-rich boundaries. With post-annealing, X atoms diffuse into amorphous boundaries and cohere with Co atoms. In addition, Co and X atoms interdiffuse around is total saturation magnetization normalized with a where is saturation magnominal volume of CoCrPt layer, and netization of CoX reacted layer. Furthermore, CoX is non-feris equal to zero. Therefore, (1) can romagnetic, namely, be rewritten in the following form: (2) Using a linear portion of the versus plot, from the intersection of the extended we can determine Authorized licensed use limited to: TOHOKU UNIVERSITY. Downloaded on October 28, 2008 at 01:49 from IEEE Xplore. Restrictions apply. ITAGAKI et al.: DIFFUSION ANALYSES OF NON-FERROMAGNETIC ELEMENT 3189 Fig. 4. Reacted layer thickness plotted against melting point of CoX compound for the post-annealed media with X cap-layer. Fig. 5. Averaged saturation magnetization plotted against enthalpy of Co-X formation for the post-annealed media with X cap-layer. line with the axis and from the gradient of the line. indicates formability of reacted layer, and a A value of value of by post-annealing is an index of exchange decoupling among ferro-magnetic grains. Therefore, we investigate the relationship between diffusion indices defined above and dominant factors of chemical coupling. plotted against the melting point of Fig. 4 shows the for the media annealed up to 420 C. CoX compound tend to have thin The media with X cap-layer of high , except for the Ta- and Nb-capped media, which form no reacted layer. This result provides us with interdiffusion mechanism around X/CoCrPt interface: Once CoX reacted layer with is formed, further interdiffusion of atoms hardly prohigh gresses due to high structural stability of CoX phase. plotted against for the Fig. 5 shows the of each annealed medium media annealed up to 420 C. is reduced from the one of nonannealed medium. In particular, of the Zr- and Hf-capped media show large reductions of is equivalent to the difficulty 99 and 130 emu/cm . of Co-X interatomic cohesion. Therefore, this result suggests not only diffuse into the grain that X atoms with low boundaries but also form lots of Co-X cohesions and make the boundaries much non-ferromagnetic. The facility of Co-X cohesion is the reason why Zr- and Hf-capped media have low diffusion temperature. Consequently, for the X-capped CoCrPt media, magnetic property and structure widely vary, depending on the chemical hardly start coupling of Co and X. The X atoms with high boundary diffusion and interdiffusion. The cap-layer with low leads into low diffusion temperature and with high into a thin reacted layer. Therefore, Hf and Zr are found to be more effective materials than Ti in this experiment from a view point of mass production. Additionally, we found that only 0.5 nm Hf cap-layer is sufficient for exchange decoupling. ACKNOWLEDGMENT The authors would like to thank N. Goto from OHARA Inc. for contributing all the glass substrates used in the experiment. REFERENCES [1] S. Saito, F. Hoshi, N. Itagaki, and M. Takahashi, “Characterization to realize CoCr-based perpendicular magnetic recording media with high squareness and normalized coercivity,” J. Appl. Phys., vol. 93, pp. 6775–6777, 2003. [2] Y. Hirayama, Y. Honda, A. Kikukawa, and M. Futamoto, “Annealing effects on recording characteristics of CoCr-alloy perpendicular magnetic recording media,” J. Appl. Phys., vol. 87, pp. 6890–6892, 2000. [3] A. G. Roy, N. T. Nuhfer, and D. E. Laughlin, “Postannealing effects on magnetic properties and microstructure of CoCrPt/Ti perpendicular recording media,” J. Appl. Phys., vol. 93, pp. 8179–8181, 2003. [4] S. Saito, N. Itagaki, and M. Takahashi, “Improvement of perpendicular magnetic properties by postannealing for M’-CoCrPt-M stacked media (M, M’ Ti, Ta, Ru, Pt, CrMn, MnSi),” IEEE Trans. Magn., pt. 2, vol. 40, no. 4, pp. 2467–2469, Jul. 2004. [5] , “Isolation of magnetic grains for CoCr-based perpendicular media with Ti cap- and under-layers through application of post-annealing,” J. Magn. Soc. Jpn., vol. 28, pp. 295–300, 2004. [6] M. Takahashi, A. Kikuchi, and S. Kawakita, “The ultra clean sputtering process and high density magnetic recording media,” IEEE Trans. Magn., pt. 1, vol. 33, no. 5, pp. 2938–2944, Sep. 1997. [7] S. Saito, N. Itagaki, F. Hoshi, and M. Takahashi, “Improvement of magnetocrystalline anisotropy of columnar structure for epitaxially grown CoCr-based perpendicular media,” J. Appl. 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