ASME/JSME Joint Conference on Micromechatronics for Information and Precision Equipment (MIPE 2006) Santa Clara, CA, June 21-23, 2006

Raman Spectroscopy and Nano Hardness Measurements of DLC Overcoats on Commercially Available Sliders and Disks R. Brunner1, A. Khurshudov2, G. W. Tyndall2, F. E. Talke1 1

CMRR, University of California, San Diego 9500 Gilman Dr. -0401, La Jolla, CA 92093-0401, USA E-mail: [email protected] 2

Samsung Information Systems America 75 West Plumeria Drive, San Jose, CA 95134, USA

Introduction Magnetic recording heads and disks are protected by a thin carbon overcoat on the order of 3nm in thickness. To achieve a storage density of 1 Tbit/inch2, a reduction in the flying height between slider and disk is required. The magnetic spacing (distance between magnetic layer on the disk and the pole piece of the read-write head) that is needed for an areal density of 1 Tbit/inch2 is on the order of 6nm [1]. At a flying height of about 3nm this implies an overcoat film thickness of 1nm each for the slider and the disk as well as a 1nm lubricant film. Film thicknesses on this order are extremely difficult to manufacture and to evaluate. Sputtering, chemical vapor deposition and arc-discharge techniques are used to deposit wear protective overcoats on disks and sliders. Depending on the technique used, the amorphitization stage in the carbon overcoat is changing from amorphous carbon (a-C) to tetrahedral amorphous (ta-C) carbon. As a consequence, the mechanical and tribological properties of the films change with the changes in the sp2 and sp3 content. Raman spectroscopy has been applied widely to determine the sp2 and sp3 content of carbon films and to obtain information about morphology and materials properties [2]. In addition, Raman spectroscopy has been used to measure the thickness of thin carbon films up to 10nm [3, 4]. To determine mechanical properties of thin carbon films, nano-indentation and nano-scratch testing are generally performed. Tribological performance of carbon films has also been investigated using scanning probe microscopy (SPM) [5]. This paper investigates structural and hardness properties of thin carbon overcoats for a number of

Corresponding author: Ralf Brunner

sliders and disks manufactured by various vendors. We first use Raman spectroscopy to identify the ratio of sp2and sp3-bonds in the carbon films to characterize the amorphitization of the films [6]. Thereafter, nanoindentation and nano-scratch testing is performed to determine mechanical properties and wear characteristics of the films. Finally, the results from the Raman and hardness measurements are analyzed to investigate whether a correlation exists between the Raman spectra and the mechanical properties of the carbon films.

Raman spectroscopy Raman spectroscopy was used to investigate the structural parameters of a number of carbon overcoats from commercially available disks and sliders. Fig. 1(a) shows Raman spectra for six disks from different vendors and Fig. 1(b) shows spectra of five sliders from different vendors. From Fig. 1(a) we observe that the Raman spectra for the disks evaluated are very similar. Well defined G-band and D-band peaks are seen for all disks investigated at wavenumbers of 1556cm-1 and 1389cm-1, respectively. The profiles of the spectra indicate that a high fraction of amorphous carbon (a-C) is present in the overcoat. The variation in the magnitude of the curves for both the disks and sliders appears to be a consequence of laser beam alignment and variations in the thickness of the carbon overcoats [3, 4]. The Raman spectra for the five sliders are shown in Fig. 1(b). We observe that the G-band is well defined for each spectrum, and that the shape of this band is similar to that found for the disks. The G-peak is present near a wavenumber of 1560cm-1 for sliders 1, 3, and 4, while it is near a wavenumber of 1530cm-1 and

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b)

a)

Fig.1 Raman spectra of different commercially available disks (a) and sliders (b) 1522cm-1, respectively, for sliders 5 and 2. For all sliders, the D-band peak is almost absent, seemingly contributing to the shift in the location of the G-band towards lower wavenumbers. The reason for the absence of the D-peak seems to be related to the tetrahedral amorphous carbon structure of the films, i.e., a higher amount of sp3-bonding is present for an increasing wavenumber [6]. Therefore, it is justifiable to suggest, for instance, that slider#4 has a higher amount of sp3-bonding than sliders #1 or #2.

Nano-indentation and nano-scratch testing To determine the qualitative hardness of the films, we have used a 2D - Lateral Force Transducer (Triboscope®, Hysitron, Inc.) combined with a Scanning Probe Microscope Stage (NanoScope®, Digital Instruments). Nano-indentation and nano-scratch testing was performed on all disks and sliders evaluated. The relative hardness was measured using nano-indentation. During nano-scratch testing, the normal force, the lateral force and the resulting friction coefficient were monitored. For both measurements, a cube corner tip was used and a maximum normal force of 70µN was applied. The contact depth on the disks at a maximum force of 70µN was approximately 8nm. For the same force, the contact depth on the sliders was approximately 3nm. In both cases, the indentation equaled or exceeded the thickness of the films. Therefore, we can conclude that the hardness measurements are affected substantially by the substrate. However, since the conditions for the

indentations were kept constant, a relative comparison between individual samples should yield acceptable qualitative results. Fig. 2a shows the hardness measured by nanoindentation and Fig. 2b the friction coefficients measured by nano-scratch testing for the six disks evaluated. Analyzing the results of the tests, we observe that both the hardness and the coefficient of friction are almost constant for all disks. The hardness data show values between 7GPa and 8GPa. The friction coefficient was found to be a slight function of the load. For a load of 70µN, a friction coefficient between 0.2 and 0.23 was measured for the various disks, while at a load of 35µN the friction coefficient decreased to a value of ~0.17. At a higher load, the indentation depth during scratching increases. Thus, it is likely that this increase causes the observed increase in the friction coefficient. Figure 3a shows nano-indentation measurements and Fig. 3b shows nano-scratch measurements on five different sliders for the same conditions. We observe that the hardness of the different sliders is nearly constant, showing a value of approximately 10GPa. This value is higher than the hardness value of the disks. Since substrate effects have a large influence on hardness measurements of these extremely thin films, the higher hardness in the case of the sliders can be correlated to the harder substrate material (Al3O2-TiC) of the sliders. In addition, the tetrahedral amorphous carbon structure of the carbon films on the sliders should give higher hardness values than those observed for the amorphous carbon films on the disks.

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a)

b)

Fig.2 Nano-hardness measurements at 70µN (a) and friction coefficient measurements at 35µN, 50µN and 70µN using nano-scratch (b) on various disks No correlation between the hardness measurements and the shift in the G-band structure for the sliders was found. The friction coefficient for the various sliders was between 0.25 and 0.4 and decreased only slightly at a lower load of 35µN. The value of the friction coefficient for slider#1 was higher compared to that of the other sliders and increased to 0.7 at an applied load of 70µN. In general, we found that the friction coefficient for the sliders increased slightly at higher loads. This effect seems to be related to adhesion and debris formation. It apparent, however, that the materials and tribological properties of the various films investigated are similar, i.e. the films manufactured by various vendors appear to be manufactured in a similar way.

Conclusions Carbon overcoats of commercially available sliders and disks from various vendors were investigated. Raman spectroscopy, nano-indentation and nano-scratch measurements were performed to characterize graphitization, hardness and friction coefficient of the carbon films. Raman spectroscopy showed that only slight differences exist in the amorphous characteristics of the carbon overcoats for the disks investigated. Somewhat larger differences were found in the characteristics of the carbon films of the various sliders investigated, seemingly related to the amount and presence of tetrahedral amorphous carbon structure in the overcoat of the sliders.

a)

b)

Fig.3 Nano-hardness measurements at 70 µN (a) and friction coefficient measurements at 35µN, 50µN and 70µN using nano-scratch (b) on various sliders Although variations in the Raman spectra of the sliders are observable, hardness and friction measurements did not show significant changes for the various sliders and disks investigated. The results suggest that the manufacturing processes used by the different vendors for sliders and disks are very similar.

References [1] D.J. Li, Y.W. Chung, “Ultrasmooth CNx Overcoats for Next-Generation Hard Disks,” IEEE Trans. Magn., Vol. 39, No. 2, 765-768 March 2003. [2] J. Robertson, “Diamond-like amorphous carbon” Materials Science and Engineering, R 37, 129-281, 2002. [3] S. S. Varanasi, J. L. Lauer, F. E. Talke, G. Wang, and J. H. Judy, “Friciton and Wear Studies of Carbon Overcoated Thin Films Magnetic Sliders: Application of Raman Microspectroscopy,” J. Trib., 119, 471, 1997. [4] T.W. Scharf, I.L. Singer, “Thickness of diamondlike carbon coatings quantified with Raman spectroscopy,” Thin Solid Films, 440, 138-144, 2003. [5] B. Jacoby, A. Wienss, R. Ohr, M. von Gradowski, H. Hilgers, “Nanotribological properties of ultrathin carbon coatings for magnetic storage devices”, Surface and Coatings Technology, 174 –175, pg.1126–1130, 2003. [6] A. C. Ferrari, “Diamond-like carbon for magnetic storage disks,” Surf. And Coat. Tech., 180-181, 190206, 2004.

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Tribological performance of carbon films has also been investigated using scanning probe microscopy (SPM) [5]. This paper investigates structural and hardness properties of thin carbon overcoats for a number of sliders and disks manufactured by various vendors. We first use Raman spectroscopy to identify the ratio of sp2 ...

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