WEAR

ELSEVIER
Wear 181-183 (1995) 743-758

Nanoindentation, microscratch, friction and wear studies of coatings for contact recording applications
Bharat Bhushan a, B.K. Gupta a, Michael H. Azarian b
Computer Microttibdogy and Contamination Department of Mechanical Engineering The Ohio State University, Columbus, OH 43210-1107, USA b Censtor Corporation, 530 Race Street, San Jose, CA 95126, USA Laboratory,

Received 29 March 1994; accepted 3 November 1994

Abstract A nanoscale monolithic slider-suspension produced by photolithography is used for contact recording. The contact pad consists of a multilayered structure consisting of Sic, amorphous hydrogenated carbon (a-C:H), AlzOs, Si, and Co-Nb-Zr films. In this study, we have compared hardness, Young s modulus of elasticity, and scratch resistance or adhesion of various coatings deposited on a single-crystal silicon wafer by nanoindentation and microscratch techniques and friction and wear performance by sliding against a diamond tip and sapphire ball in reciprocating mode. Sic coatings exhibit the highest hardness, about 27 GPa, and the highest elastic modulus, about 255 GPa. Microscratch data indicate that SiC and a-C:H coating exhibit the highest resistance to scratching or debonding from the substrate. During scratching, an A&O, coating deforms like a ductile metal rather than like a ceramic. Si and Co-Nb-Zr coatings exhibit ploughing of the tip into the sample surface and debris generation right in the beginning of the scratch. Sic coatings exhibit the best wear performance against a diamond tip as well as a sapphire ball. For comparisons, we also made mechanical property measurements on bulk materials used in

conventional recording: Ni-Zn ferrite, Al,O,-Tic, and Sic (under development). The bulk Ni-Zn ferrite sample was found to be damaged by grain pull-out during scratching even at a low load of 3 mN. Bulk Al,O,-TiC exhibits unexpected ploughing of the sample right from the beginning of the scratch. Bulk Sic did not exhibit any signs of significant damage up to a normal load of about 15 mN. Overall comparison of mechanical properties of bulk materials and coatings suggest that Sic is the most desirable coating in the contact pad for low wear. An Sic coating is also recommended as an overcoat for thin film
magnetic
Keyword:

disks. Contact recording; Nanoindentation; Microscratch

1. Introduction The magnetic recording process involves storage and retrieval of information on a magnetic medium undergoing relative motion in close proximity to a magnetic head. In conventional magnetic rigid disk drives, a head slider containing the read-write element is loaded against the rotating disk medium to about 100 mN. Under steady state operating conditions, a hydrodynamic air bearing develops which lifts the slider off the disk surface at velocities exceeding about 1 m s- . Direct sliding contact between slider and disk occurs during drive starts and stops, and intermittently during normal operation due to disturbances of the air bearing. In order to enable continued increases in storage density, head-disk separation (i.e. flying height) must be minimized and ideally reduced to zero [l]. While a contact recording device would be highly attractive from the

perspective of magnetic performance, tribological issues have to date discouraged their introduction into commercial drives. A number of contact recording devices are currently under development within the storage industry. One of the most advanced designs, the Censtor MicroFlexhead (referred to hereafter as the microflex head), is an integrated head/flexure/conductor structure which is substantially smaller than the conventional head [2,3]. This device is designed to operate in continuous sliding contact with the disk surface, at linear velocities of 3-8 m s-l. A single-pole perpendicular-probe-type transducer provides tolerance to as much as 7 pm of vertical pole tip wear without significant signal degradation, whereas allowable head wear for the MRtype thin film head is only about 3 pm and for the inductive-type thin film head it is 2-3 times that of the MR heads. The pole is embedded in wear-resistance

Elsevier Science S.A.

SSDI 0043-1648(94)07101-2

B. Bhushan

et al. I Wear 181-183

(1995) 743-758

Fig. 1. Schematic of a perpendicular probe-type head on the end of a flexure beam (microflex head) with layered pancake coil, conductors and bonding pads, and a contact pad of about 20 pmX36 pm-

Fig. 2. Schematic layout of various coatings used in the microflex head contact pad and pole structure.

amorphous hydrogenated carbon (a-C:H), which forms a contact pad with nominal length, width, and thickness (height) of 20 pm, 36 pm, and 7-9 pm, respectively. In order to achieve low stiction and low head wear, the slider suspension mass, foot print of the contact pad, and the normal load are reduced by two or three orders of magnitude from current designs. In the first generation microflex head design, a read-write transducer is fabricated at one end of a rectangular (30 pm thick) sputtered amorphous alumina flexure beam. The beam, schematically illustrated in Fig. 1, contains two parallel copper leads connecting the read-write element at the free end to bonding pads at the other end. The integrated transducer/suspension structure is non-gimbaled, requiring appropriate mounting and alignment of the beam. The length, width, and thickness of initial configurations of the flexure beam are 10 mm, 500 pm, and 30 pm, respectively. The spring constant is about 0.6 N m- , and the effective mass is approximately 600 pg. A perpendicular-probetype head, with a flux return pole and multilayered pancake coil, is fabricated using photolithographic techniques in the end of the beam. The main pole and front yoke reside on the vertical end of the beam, and are covered with a layer of a-C:H. This configuration minimizes sensitivity to head wear and ensures negligible air bearing lift of the flexure beam. Typical applied normal loads are about 40 mgf. The pole material is an ion-beam-sputtered Co-Nb-Zr alloy of about 275 nm thickness, surrounded on both sides by about 200 nm of r.f.-sputtered alumina. There is also an r.f.-sputtered Sic adhesion layer of about 70 nm thickness between the r.f.-plasma-enhanced-chemical-vapour-deposited amorphous carbon wear pad and the alumina. On the side nearest the free end of the beam, there is an r.f.-sputtered Si adhesion layer of about 100 nm between the alumina and the carbon. The progression of layers in a-C:H,

Sic, Al,03, Si, and a-C:H, going from the leading edge to the trailing edge of the pad (Fig. 2). With the head in continuous sliding contact with the rotating disk surface, wear and failure mechanisms may be expected to be different than those observed in conventional flying head-disk interfaces. The propensity toward catastrophic failure (head crash) is removed with the elimination of the air bearing [2]. Sliding wear mechanisms which are potentially operative in contact recording are more sensitive to mechanical properties of the materials at the interface, such as shear strength, hardness, elastic modulus, and fracture toughness. In this study, the objective is to compare the micromechanical and tribological properties of various coatings present in the thin film contact pad. For comparisons, we also present the mechanical property measurements of bulk head slider materials used today in conventional recording [l].

2. Experimental techniques Coatings of Sic, a-C:H, A&,0,, Si, and Co-Nb-Zr used for head construction were deposited individually on single-crystal Si (100) wafers. Sic and Si were deposited by r.f. sputtering in pure Ar atmosphere from 0.203 m diameter targets in static mode. a-C:H was deposited using r.f. plasma-enhanced chemical vapor deposition (PECVD) in a planar powered electrode system. Al,O, was deposited by r.f. sputtering in pure Ar atmosphere from a 0.225 m diameter Al,O, target. Co-Nb-Zr was deposited by argon ion beam sputtering from a target of the desired composition. Deposition techniques and thicknesses of samples used in this study are summarized in Table 1. The a-C:H coatings were deposited in two thicknesses in order to study the effect of thickness on the mechanical properties. These coatings were characterized by their hardness, Young s modulus of elasticity (elastic modulus), and scratch resistance using a nanoindentation and microscratch apparatus at low loads of a few millinewtons. In order

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Table 1 Deposition coatings Coating

90% unloading;
techniques deposited and thicknesses of individual contact pad on single-crystal Deposition process R.f. R.f. R.f. R.f. Ion sputtering PECVD sputtering sputtering beam sputtering Si( 100) Thickness (nm) 400 400,500O 400 400 270

Sic a-C:H J&D, Si Co-Nb-2x

reloading to peak load; holding the indenter at peak load; finally unloading completely. Multiple loading and unloading steps were performed to examine the reversibility of the deformation, thereby making sure that the unloading data used for analysis purposes were mostly elastic. The first hold step was included to incorporate the corrections due to thermal drift. The second hold step was included to avoid the influence of creep on the unloading characteristics.

2.2. Scratch resistance by microscratch

Table 2 Reported mechanical properties of bulk materials, used in this study in the coating or bulk form, measured by conventional techniques Bulk material Microhardness @Pa) Elastic modulus @Pa) Sic ALO3 Single-crystal Si(100) Ni-Zn ferrite Al,OJ-Tic a 23 21 9-10 6.9 22.6 425 390 188 122 450 Flexural strength (MPa) 650 500-600 150 880 Fracture toughness (MPa mm) 4.0 4.9 0.7 1.0 -

a 70wt.%A1203-30wt.%TiC.

to compare the mechanical properties of coatings with those of bulk ceramics commonly used for air bearing head slider construction for conventional recording, nanoindentation and microscratch measurements were also made on bulk Ni-Zn ferrite, Al,O,-Tic, and Sic materials (under developments as a slider material). Mechanical properties of bulk materials used in this study in either coating or bulk form, measured by conventional techniques, are summarized in Table 2. Friction and wear properties of various coatings and bulk silicon were compared by sliding coated coupons against a diamond tip and a single-crystal sapphire ball under ambient conditions. 2.1. Hardness and elastic modulus by nanoindentation Hardness and elastic modulus are calculated from the load vs. displacement data obtained by nanoindentation on each coating and bulk material at six different peak indentation loads ranging from 0.08 to 15 mN using a commercially available nanoindenter apparatus. This instrument monitors and records the dynamic load and displacement of a three-sided pyramidal diamond (Berkovich tip with a radius of about 100 nm) indenter during indentation with a force resolution of about 75 nN and displacement resolution of about 0.1 nm. In the present studies, a typical indentation experiment consists of seven subsequent steps: approaching the surface; loading to peak load; unloading 90% of peak load; holding the indenter after

In microscratch studies, a conical indenter is drawn over the sample surface with ramping up of the load until damage occurs; the load corresponding to this damage provides a measure of scratch resistance or adhesive strength of a coating and is called the critical load. The definition of damage can be the onset of cracking around the scratching tip, spalling of the coating, or the formation of a channel in which all of the coating has been removed from the substrate. The scratching process consisted of two operations: normal indentation carried out by an indenter assembly, and the translational motion of the sample by a motorized x-y-z stage. The friction force or tangential force, acting opposite to the sample movement, was obtained by measuring the lateral deflection of the scratch tip holder using a capacitance proximity probe. The coefficient of friction during scratching was calculated by dividing the friction force by the normal load. A sudden or steady increase in the coefficient of friction was related to damage. Scratches were made by translating the sample while ramping the loads on the conical diamond tip (1 pm tip radius) over different load ranges from 2 to 25 mN. A typical scratch experiment consisted of four subsequent steps: approaching the surface; indenting the sample surface by loading the tip to 2 mN; translating the sample at ramping load to a load ranging from 4 to 25 mN at a speed of 5 pm s- ; final unloading of the tip. In the present study, we made 500 pm long scratches each at loads of 2-4, 2-6, 2-10, 2-15, 2-20, and 2-25 mN. Relatively high stresses during scratching were chosen as compared to the typical stresses in an asperity contact, in order to induce failure in a single scratch. It is noted that much of the catastrophic damage in the lightly loaded contact recording devices occur from isolated incidences of high loading and/or threebody abrasion involving high contact stresses. During scratching, scratch-induced damage, specifically fracture or delamination, of a coating were monitored by in situ tangential (friction) force measurements and by optical and scanning electron microscopy (SEM) imaging of the scratches after testing. The damage events of fracture or delamination of a film during scratching were correlated to abrupt increases in the coefficient of friction.

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B. Bhushan et al. / Wear 181-183

(1995) 743-758

747

and second loading steps of the indentation. Pop-in marks in the loading curves result from sudden penetrations of the tip into the sample. A non-uniform penetration of the tip in coatings with submicrometer thicknesses probably results from either onset of plastic deformation of formation of cracks [4] or from debonding or delamination of the coating from the substrate. The a-C:H coating exhibits only one pop-in mark at about 0.15 mN indentation load, while all other coatings and bulk Si exhibit several pop-in marks at lower indentation loads. The pop-in mark in a-C:H at a higher load of about 0.15 mN suggests that it probably has the highest resistance to crack formation or to debonding from the substrate. Pop-in marks in the loading curve of bulk Si appear right at the beginning at about 0.02 mN indentation load; this may be due to microcracking because of the low fracture toughness (0.7 MPa ml). Significant hysteresis in two cycles of loading and unloading of the silicon substrate is due to a pressure-induced phase transformation from its normal diamond cubic form to the p-Sn phase [5]. Based on the occurrence of pop-in marks during loading, it appears that the a-C:H coating is the most resistant to crack formation or to debonding from the substrate. Hardness and elastic modulus profiles as a function of indentation depth for various coatings and singlecrystal silicon are shown in Fig. 5. Hardness and elastic

modulus data of various coatings and bulk materials at low and high indentation depths are summarized in Table 3. Indentation depths obtained at minimum and maximum indentation loads are also included in this table. Hardness and elastic modulus values at lower indentation depths of about lo%-30% of the coating thickness correspond to the coating and values at higher indentation depths indicate composite values of the coating and the silicon substrate. The Sic coating exhibits the highest hardness of about 27 GPa and elastic modulus of about 255 GPa among the coatings examined. The a-C:H coating exhibits a hardness of about 14 GPa and elastic modulus of 115 GPa. The thickness of the a-C:H coating significantly affects its hardness and elastic modulus. Thick a-C:H coatings are harder (18 GPa, hardness profile not shown) than thinner coatings (14 GPa). This difference in hardness is probably due to changing growth characteristics as coating thickness increases during deposition of the a-C:H coating. A&O, and Co-Nb-Zr coatings exhibit lower hardnesses of about 8 GPa. The hardness of the silicon film (12 GPa) is very close to that of single-crystal silicon. However, the elastic modulus of the silicon film is found to be lower (140 GPa) than that of single-crystal silicon (220 GPa). In general, hardness and elastic modulus of coatings are strongly influenced by their crystalline structure,

30,
Si

coating

,300 _a

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Depth, nm
a-C:H

50

100

150

200

2;.0 ti

300 a _&

Depth, nm Co-Nb-21 __ 30a$

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loo

150

200

250

01. 0

50

Depth, nm

100

150

200

250 O a

Depth, nm
silicon. These values are calculated

modulus profiles with indentation depth for various coatings and single-crystal data generated at six peak loads ranging from 0.08 to 15 mN.

748
Table 3 Hardness Material type Coating Sic a-C:H (400 nm) a-C:H (5000 nm) AW3

B. Bhushan et al. / Wear Mi-183 (lP#)

743-758

and elastic

modulus Material

of various

coatings

and bulk materials Indentation depth (nm) 20 180 17 270 16 260 30 240 28 220 30 235 16 270 21 250 13 160 12 145

obtained

by nanoindentation Load (mN) 0.2 10 0.08 15 o.otd 15 0.2 10 0.2 10 0.2 10 0.08 15 0.2 15 0.2 15 0.2 15

at loads Hardness (GPa) 27.0 25.0 14.0 15.0 18.0 15.0 g.3 10.6 12.0 13.0 8.0 9.0 11.0 11.7 14.0 12.0 32.0 35.0 40.0 38.0

ranging

from 80 PN to 15 mN Elastic (GBa) 255 210 115 125 140 170 140 170 140 160 200 220 220 240 210 a 220 b 450 d 520 480 480 g modulus

Si Co-Nb-Zr Bulk Single-crystal Si( 100) Ni-Zn ferrite A1203-Tic Sic

a b = f r

At 10 nm depth. b At 120 nm depth. c 7Ov&%-3Owt.%. At 12 nm depth. At 130 nm depth. f At 8 nm depth. g At 110 nm depth.

microstructure, stoichiometry, and growth characteristics which usually depend on the deposition parameters [6]. Sic coatings with different phases, namely &iC and P-Sic, and carbon contents exhibit large variations in their hardness. For instance, Brutsch [7] reported an increase in hardness of chemical-vapor-deposited Sic coating from 10 to 30 GPa with an increasing carbon content from 0 to 30% which corresponds to the stoichiometric composition. Amorphous hydrogenated Sic coatings deposited by PECVD at 175 C and 600 C substrate temperatures exhibit hardnesses of about 17 GPa and 46 GPa and elastic modulus of about 90-145 GPa and 240 GPa, respectively [8]. Mechanical properties of a-C:H coatings have been known to change over a wide range with sp3-to-sp bonding ratio and amount of hydrogen. Hydrogen is believed to play a crucial role in the bonding configuration of carbon atoms by helping to stabilize tetrahedral coordination (sp bonding) of carbon atoms. Sawides and Bell [9] reported an increase in hardness from 12 to 30 GPa and elastic modulus from 62 to 213 GPa with increasing sp3-to-sp bonding ratio, from 3 to 6, for a a-C:H coatings deposited by low-energyion-assisted unbalanced magnetron sputtering of a graphite target in an Ar-H, mixture. Bhushan et al. [lo] reported hardnesses of about 15 GPa and 35 GPa

and elastic moduli of about 140 GPa and 200 GPa, measured by nanoindentation, for a-C:H coatings deposited by d.c. magnetron sputtering and r.f. PECVD techniques, respectively. High hardness of r.f. PECVD a-C:H coatings was attributed to a higher concentration of sp3 bonding than in a sputtered a-C:H coating. Cho et al. [ll] and Rubin et al. [12] observed that the hardness decreased from 15 to 3 GPa with increasing hydrogen content. Bhushan and Doerner [13] reported hardness of about 10-20 GPa and elastic modulus of about 170 GPa, measured by nanoindentation, for 100 nm thick d.c.-magnetron-sputtered a-C:H on the silicon wafer. White et al. [14] reported hardness as high as 18 GPa, measured by nanoindentation, for 120 nm thick sputtered carbon coating on 40 nm thick Co-Pt-Cr alloy coating over an Al-Mg/NiP disk. Dekempeneer et al, [15] reported hardness of about 13 GPa and elastic modulus of about 130 GPa, measured by nanoindentation, for 1.7 pm thick r.f. PECVD a-C:H coatings deposited on Si. The hardness (14 GPa) and elastic modulus (115 GPa) of our a-C:H coating are close to the values reported by Cho et al. [ll] and Dekempeneer et al. [15]. Alz03 coatings can be deposited by sputtering in a number of metastable polymorphs in addition to the thermodynamically stable cu-A&O, by choosing appro-

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priate substrate temperatures [16]. Microhardness of A&O, coatings was found to be strongly affected by the microstructure of the coating. For instance, amorphous and (Y-A&O, coatings deposited by r.f. sputtering at substrate temperatures of less than 400 C and greater than 1000 C exhibit hardnesses of 4 GPa and 10 GPa, respectively. We examined the crystallinity of our sputtered Al,O, coatings by X-ray diffraction and found that coatings were amorphous which explains the lower hardness values. 3.1.2. Scratch resistance In the present study, 500 pm long scratches were made at six different ranges of ramping loads in order to identify the normal load necessary to damage the coating. Friction profiles and SEM images of scratches made at 2-25 mN normal load on various coatings and single-crystal silicon are compared in Figs. 6 and 7. We note that damage during scratching at normal load of 2-25 mN was least to Sic. Coefficients of friction and critical load for the various coatings and singlecrystal silicon are summarized in Table 4. Coefficients of friction of all films during scratching are comparable,
SIC g .d 0.8

although the critical load for SIC coating is lower than that with an a-C:H coating, but damage to an a-C:H coating is higher than that of Sic coating. The coefficient of friction of about 0.27 between the diamond tip and Sic coating during scratching does not vary significantly with increasing load below the critical load (Fig. 6). However, it increases to 0.60 after normal load exceeds the critical load of about 15 mN. In the friction profiles several bursts (instantaneous increase in friction) are present when normal load exceeds 10 mN (Fig. 6). These bursts in friction indicate that the coating has experienced some sort of damage. SEM images of various regions of a scratch made at 2-20 mN are shown in Fig. 8. We note from the SEM image shown below the friction profile that each burst in the friction profile corresponds to formation of debris. It is obvious from the SEM images shown on the top of the friction profile that the Sic coating was damaged incrementally with increasing load. There is no evidence of any delamination of coating from the silicon substrate in the image of region B or any severe damage even at 25 mN load.
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Fig. 6. Coefficient of friction profiles as a function of ramping normal load for 500 pm long scratches made at 2-2.5 mN on various coatings and single-crystal silicon. An abrupt increase or a burst in the friction profile is associated with a damage event occurring as a result of scratching. The normal load corresponding to an abrupt increase in friction or onset of damage on the surface is defined as the critical load. Si and Co-Nb-Zr coatings do not show an abrupt increase in friction because of ploughing of the tip into the coating right in the beginning of the scratch.

750

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Fig. 9. SEM images of various region and coefficient of friction profile of a 500 wrn long scratch made on a-C:H coating at 2-25 mN. Abrupt increase in friction at about 18 mN normal load is associated with severe damage to the coating. The image of region C shown on the top clearly shows some cracks in the coating.

Fig. 7. Comparisons of SEM images of scratches (last 120 Km towards the end) made at 2-25 mN on various coatings and single-crystal silicon.

Fig. 8. SEM images of various regions and coefficient of friction profile of a 500 pm long scratch made on Sic coating at 2-20 mN. Each burst in the friction profile is found to be associated with the formation of debris. No significant damage occurs between two bursts in the friction profile. Furthermore, no cracking or delamination is visible even at 20 mN normal load.

Scratching of the a-C:H coating exhibits an increase in coefficient of friction from 0.10 to 0.30 with increasing load until the coating was damaged. Damage of the coating at about 18 mN results in an increase in the coefficient of friction to 0.40. SEM images of various regions of a scratch made at 2-25 mN are shown in

Fig. 10. SEM images of (a) various regions and coefficient of friction profile of a 500 pm long scratch made on AIZO, coating at 2-15 mN and (b) two typical chips of debris generated during a scratch on AlzOs coating. An increase in friction at about 6 mN is associated with the generation of debris. Some debris consisting of curly chips is formed even at 4 mN, shown in the image of region A. Abrupt increase in friction to 0.6 at about 12 mN normal load resulted in formation of debris of submicrometer size. The SEM images at high magnification shown in (b) clearly show a twist in the chips, indicating significant plastic deformation.

B. Bhwhan

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Table 4 Coefficient at ramping Material type

of friction loads

and critical

load mN

for various

coatings

and bulk silicon,

esimated

from an abrupt

increase

in friction

during

scratching

of Z-4 and 2-25 Material

Ramping load range (mN)

Critical

load

(mN)

Coefficient At beginning

of friction

during

scratch At end

Coating

Sic a-C:H (400 nm) AU% Si coating

2-l 2-25 2-4 2-25 2-4 2-25 2-4 2-25 2-4 2-25

No damage 15 No damage 18 No damage 6-12 Ploughing of coating from beginning of scratch Ploughing of coating from beginning of scratch

0.20 0.25 0.20 0.12 0.10 0.15 0.45 0.35 0.25 0.50

0.20 0.70 0.10 0.50 0.10 0.50 0.18 0.30 0.40 0.30

Co-Nb-Zr

Bulk

Single-qstal Si(100) Ni-Zn ferrite Al&-Tic

2-4 2-25 2-4 2-25 2-4 2-25 2-4 2-25

4 (onset of ploughing) 16 (onset of fracture) No damage 10 Ploughing of sample from beginning of scratch No damage 15

0.05 0.10 0.10 0.10 0.10 0.15 0.12 0.12

0.10 0.80 0.35 0.80 0.20 0.30 0.50 0.75

Sic

Fig. 9. No formation of debris or any significant damage to the a-C:H coating is apparent below 18 mN. However, after exceeding 18 mN normal load, the coating was severely damaged and a large quantity of debris was formed (see images of regions C and D). Furthermore, SEM imaging at high magnification (top image of region C) clearly indicates the generation of cracks in the coating. In contrast to the Sic coating, although the a-C:H coating exhibits a lower coefficient of friction and higher critical load, the severity of damage is greater after the critical load limit of 18 mN is exceeded. Wu [17] has made scratches with a conical tip of 1 pm tip radius on two 110 nm thick amorphous carbon coatings deposited on Si by a d.c. planar magnetron sputtering process at 30 and 6 mTorr Ar sputtering pressure and 20 nm thick r.f.-sputtered hydrogenated carbon coating. He observed damage on the d.c.-sputtered coating, deposited at 30 mTorr Ar sputtering pressure, at a low normal load of about 3 mN and on the coating deposited at 6 mTorr Ar sputtering pressure, at a normal load of about 32 mN. The r.f.-sputtered hydrogenated carbon coating was also damaged at about 3 mN normal load. It was noticed that the carbon coating wore but it still adhered to the plastically deformed substrate. There was a sudden increase in scratch width at 3 mN. We have also observed similar trends of sudden damage, after exceeding critical load, of our a-C:H coating. However, the critical load was higher

(about 18 mN) probably because of its higher thickness (400 nm). The Al,O, coating exhibits a low coefficient of friction of about 0.15 below the critical load. In some scratches, we have noticed an instant increase in coefficient of friction to about 0.3 for a short period which again dropped to 0.2 and remained constant up to a critical load limit of about 12 mN (Fig. 10). We note from the images of various regions of scratches that normal load of about 6 mN causes only minor damage to the coating. However, the coating was severely damaged after the normal load exceeded 12 mN. SEM images of various regions of a scratch made at 2-15 mN and debris generated during scratching are shown in Fig. 10. The image of region A at a low load of 4 mN at low magnification, shown below the friction profile, clearly shows the formation of curly chips which are commonly formed in a ductile material. A twist in a typical chip of debris can be clearly seen in the lower image of Fig. 10(b). From the appearance of curly chips in the debris (Fig. 10(b)), it is concluded that the r.f.sputtered Al,O, coating probably behaves here like a ductile metal rather than a brittle ceramic. In Si coatings, the coefficient of friction first decreases from 0.43 to 0.15 and then increases to 0.35 with increasing normal load. SEM images of various regions of a scratch made at 2-10 mN are shown in Fig. 11. An SEM examination of the entire scratch (image not

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Fig. 11. SEM images of various regions and coefficient of friction profile of a 500 pm long scratch made on Si coating at 2-10 mN. Ploughing of the coating and plastic flow of material along the scratch track right at the beginning of the scratch is observed.

was formed on the side of the scratch. Further SEM examination of scratches (images not shown) indicate that probably the tip had penetrated through the coating right in the beginning of the scratch and continued scooping the coating material toward the end of the scratch. Comparisons of SEM images of debris generated in scratches on alumina and Co-Nb-Zr coatings, shown in Figs. 10 and 12, indicate significant differences in the type and nature of the debris. Bulk Si exhibits a very low coefficient of friction of 0.05 at the beginning of a scratch at 2 mN. The coefficient of friction remains constant up to 4 mN. The coefficient of friction increases abruptly from 0.05 to 0.15 and then gradually increases to 0.25 as the normal load increases from 4 to 18 mN and to 0.9 when the load exceeds 18 mN. SEM images of the scratch shown in Fig. 13 indicate that the tip started ploughing into the material right after 4 mN. The severity of ploughing increased (region B and C) with increasing load. The material fails catastrophically (region D) when the load exceeds 18 mN. Particulate debris of submicrometer size was observed when the normal load exceeded 18 mN. All samples exhibit higher coefficients of friction during scratching as compared to normal sliding against blunt samples (data to be presented later). However, in some cases coefficients of friction at low loads of about 2-4 mN during scratching are comparable to those observed in normal sliding. A higher coefficient of friction in scratching is attributed to larger contributions to friction from the ploughing component in scratching as compared to normal sliding. Sic and aC:H coatings exhibit higher scratch resistance as com-

Fig. 12. SEM images of various regions and coefficient of friction profile of a 500 pm long scratch made on Co-Nb-Zr coating at 2-25 mN. The image shown below the friction profile indicates that the tip had penetrated through the coating right at the beginning of the scratch and continued scooping the coating material toward the end of the scratch.

shown) indicates that this coating was damaged by ploughing (Fig. 7) and the amount of debris and width of scratch increased with increasing normal load. Ploughing of the coating and plastic flow of material along the scratch track right at the beginning of the scratch could be clearly seen. The Co-Nb-Zr coating does not exhibit significant variations in coefficient of friction of about 0.40 with increasing normal load. SEM images of various regions of a scratch made at 2-25 mN are shown in Fig. 12. The image of scratches shown below the friction profile in Fig. 12 shows formation of a big spiral-shaped chip at the end of the scratch. Images shown above the
friction mofile indicate that verv little particulate debris

Fig. 13. SEM images of various regions and coefficient of friction profile of a 500 Mm long scratch made on single-crystal bulk silicon at 2-20 mN. An increase in friction coefficient from 0.05 to 0.15 is associated with ploughing and results in the formation of debris of submicrometer size. An abrupt increase in friction coefficient to 1 is associated with severe damage and formation of particles of about 1 pm.

B. Bhushan et al. / Wear 181-183 (1995) 743-758

753

pared to other coatings. There is a localized fracture of Sic coating at loads of 15 mN and higher. No crack formation on a macroscale or debonding from the substrate is observed in the Sic coating even at a scratching load of 25 mN. a-C:H coatings exhibit debris formation and crack formation in the coating at 18 mN normal load. The coating is delaminated and wear debris is formed when the normal load exceeds 18 mN. The damage on Sic coatings during scratching at identical loads is considerably lower than on a-C:H coatings. In contrast, very little debris is observed with an Sic coating even at a high load of 25 mN. AlzO, coatings are damaged at about 13 mN load and formation of ductile chips is observed. The Si and Co-Nb-Zr coatings exhibit ploughing from the beginning of scratching at 2 mN with increasing width of the scratch with ramping load. In order to further understand the damage that occured during scratches made on Sic and a-C:H coatings, we have measured the depth of scratches with increasing normal load by atomic force microscopy @FM). AFM images of two regions on scratches made at 2-25 mN normal load on Sic and a-C:H coatings are shown in Fig. 14. We note that the depths of scratches on Sic coatings up to 11 mN normal load are comparable to those on a-C:H coatings. However,

after exceeding a 16 mN normal load the depth of a scratch on a Sic coating is considerably lower than on an al-C:H coating. Variations in depth of scratch with increasing normal load for Sic and a-C:H coatings are compared in Fig. 15. It is obvious from the abrupt increase in the depth of scratch that the a-C:H coating was damaged suddenly while the Sic coating was damaged gradually. Furthermore, after exceeding a critical load the scratch depth in a-C:H was higher than its thickness which indicates that this coating was removed and the tip penetrated through it and began to plough the silicon substrate. AFM data suggest that the scratch resistance and/or adhesion of an SIC coating is superior to that of an a-C:H coating. We now examine a model for scratch adhesion. During a scratch, a shear force is transmitted through the coating at the interface by elastic and plastic deformation. Bull et al. [18] have derived an expression for the critical load. They assumed that the measured friction force is the linear sum of all components due to ploughing, adhesion, and residual stress (internal). The friction force was converted to the shear stress acting on the surface layer by dividing by the crosssectional area of the track. They derived the expression for the shear in terms of work of adhesion by modeling the adhesion behavior in terms of the strain energy

f
N

H
::

(b)

(4

Fig. 14. AFM images (a) of a region which corresponds to normal load of 11 mN over a scratch on Sic, (b) of a region which corresponds to normal load of 16 mN over a scratch on Sic, (c) of a region which corresponds to normal load of 11 mN over a scratch on a-C:H coating, and (d) of a region which corresponds to normal load of 16 mN over a scratch on a-C:H coating made at 2-25 mN normal load.

754

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800

0 5 10 15

SIC
20

Normal load, mN
Fig. 15. Variation in the depth of a scratch (measured by AFM imaging) as a function of increasing normal load, made at 2-25 mN normal load on Sic and a-C:H coatings.

released during the removal of the coating. Finally the friction force was expressed in terms of normal load times the coefficient of friction. The expression for the critical load was derived by Bull et al. [18] as L = --A EW, lR c v,p., ( t 1 where A is the cross-sectional area of the scratch, E and V, are the elastic modulus and Poisson s ratio of the coating, t is the thickness of the coating, W, is the work of adhesion of the coating to the substrate ( = -yc+ x- y_; y= and x are surface free energies of coating and substrate, respectively; y= is the interfacial energy), and I.L, is the coefficient of friction at the critical load. The preceding equation suggests that the critical load is influenced by thickness, elastic modulus, Poisson s ratio, the work of adhesion of coating material, and the coefficient of friction between the coating and the indenter. Furthermore, the critical load increases with an increase in elastic modulus and a decrease in coefficient of friction. Thus it appears that higher critical loads for Sic and a-C:H coatings as compared to other coatings may be due to the high elastic modulus (255 GPa) of the Sic coating and low coefficient of friction (0.12) of the a-C:H coating. Other coatings exhibit lower critical loads because of lower hardness and elastic modulus and high coefficient of friction. 3.1.3. Friction and wear properties Coefficients of friction and wear behavior of various coatings and single-crystal silicon against a diamond tip and single-crystal sapphire ball are summarized in Table 5. Optical images of wear tracks formed on various coatings and single-crystal silicon when slid against a sapphire ball for 2 h are compared in Fig. 16. The following observations are made from the friction and wear data presented in Table 5 and Fig. 16. The Sic coating exhibits the lowest friction of about 0.06 and 0.15 against a diamond tip and sapphire ball,

a-C:H

Fig. and ball and even

16. Optical images of wear tracks formed on various coatings single-crystal silicon sliding against (a) single-crystal sapphire at 10 mN for 2 h under ambient temperature of about 22 C humidity of about 45%&S%. No wear track was found on Sic after 2 h sliding against the sapphire ball.

respectively. No wear track could be found on the Sic coating even after 2 h of sliding against either a diamond tip or sapphire ball. All other coatings exhibit a higher coefficient of friction of about 0.09 against a diamond tip. Al,O,, Si, and Co-Nb-Zr coatings exhibit some generation of wear debris when slid against a diamond tip. a-C:H, Si, and Co-Nb-Zr coatings exhibit similar values of coefficient of friction of about 0.15 when slid against a sapphire ball. The a-C:H coating did not exhibit any debris when slid against a diamond tip but little debris was observed when slid against a sapphire ball. The Al,O, coating exhibited the highest coefficient of friction of about 0.33 when slid against a sapphire ball. Si and Co-Nb-Zr coatings slid against a sapphire ball exhibit high wear and generate lots of debris compared to other coatings. The various coatings can be ranked, on the basis of low friction and wear, as Sic > bulk Si > a-C:H > Al,O, > Si coating > Co-Nb-Zr. The Sic coating exhibits the best wear performance against a diamond tip as well as against a sapphire ball, compared, to other coatings and single-crystal silicon. In general, wear performance of a coating is

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Table 5 Friction and wear of coatings slid against L natural diamond tip and sapphire ball at normal load of IO mN, sliding speed of 0.7 mm ambient temperature of 22* 1 C, relative humidity of 45% f5%, and test duration of 2 h Coating or substrate Slid against natural diamond tip PinC fin. * Observations of wear track No wear No wear Low wear Low wear Law wear No wear Slid against sapphire ball b Pi P?i

S- ,

Observations of wear track No wear Very low wear Medium wear High wear High wear Low wear

Sic a-C:H Al203 Si coating Co-Nb-Zr Bulk Si (100)

0.06 0.08 0.09 0.09 0.13 0.05

0.06 0.08 0.08 0.09 0.09 0.05

0.19 0.15 0.30 0.16 0.14 0.15

0.15 0.15 0.33 0.15 0.19 0.10

a 20 pm tip radius. b3 mm diameter. c Initial coefficient of friction. Final coefficient of friction. Yn the optical microscope.

Ni-Zn Ferrite 0.3 y o 31------

Al203-TiC 0.3 0.2 !z 3 0.1 s

Sic

O,.

10 15 20 Displacement, nm

25

0 31

10 15 20 Displacement, nm

25

0.0 _ 0 31

/f/+( ..j,, , . I
5 10 15 20 Displacement, nm 25 0 20 40 60 80 Displacement, nm 100

g
s

,... j,,,,__.: .J
,..g

.,.

l0, 0 _. 1 20

>~,../ ~ ,. . 40

J .j,:.... ,.*,.. 1 : , 60 80 nm

100

20

Displacement,

40 60 80 Displacement, nm

100

Oo

100

200

300 Displacement, nm Displacement, nm

Displacement, nm

Fig. 17. Representative load-displacement plots for Ni-Zn ferrite, Alu203-Tic, and Sic bulk materials, obtained by nanoindentation at 0.2, 2.5, and 15 mN peak indentation loads. Locations on loading culyes marked by arrows show a sudden penetration or pop-in of the tip into material during the loading step in the indentation process. Loading and unloading curves in an indentation at 0.2 mN in Sic follow nearly the same curve, indicating that deformation was mostly elastic.

significantly influenced by its hardness and elastic modulus, adhesion to substrate, and coefficient of friction. High wear performance of the Sic coating is attributed to its highest hardness and scratch resistance or adhesion.

3.2. Bulk slider materials

In this section, we present hardness, elastic modulus, and scratch and adhesion data for Ni-Zn ferrite,

156

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Ni-Zn Ferrite

m
8

Ni-Zn Ferrite (

40 -

0-o 0

50

100

150

200

250

5 I&Ll load!ti

20 A1203-TiC

25

Depth, nm

c 0.8 .s { s 0.4 .9 4
V

~01 ~ ~ . . I 0 5 10

15 Normal load, mN

20 Sic

25

.z

0.8 -

3 % E .$ 0.4 5
V

. ..~~.... ~.~.~(...I..~.~.... .~.~

0 80 100 120 140

20

40

60

10

1.5

J
20 25

Normal load, mN Fig. 19. Coefficient of friction profiles as a function of ramping normal load for 500 pm long scratches made at 2-25 mN on NM% ferrite, Al,O,-Tic, and Sic bulk materials.

Depth, nm

Fig. 18. Hardness and elastic modulus profiles with indentation depth for Ni-Zn ferrite, Al,O,-Tic, and Sic bulk materials. These values are calculated from the load-displacement data generated at six peak loads ranging from 0.2 to 15 mN.

Al,O,-Tic, and Sic bulk materials, commonly used as substrates for construction of head sliders. 3.2.1. Hardness and elastic modulus Representative load-displacement plots of indentations made at 0.2, 2.5, and 15 mN indentation loads in Ni-Zn ferrite, A&O,-Tic, and Sic are compared in Fig. 17. Ni-Zn ferrite exhibits several pop-in marks right from the beginning of loading in indentation at very low loads of about 0.02-1.2 mN. The pop-in mark at 0.12 mN, shown by the larger arrow on the top load-displacement curves of Ni-Zn ferrite in Fig. 17, corresponds to an inward jump of the tip by about 2 nm. This jump probably indicates a transition from elastic to plastic deformation. Other pop-in marks corresponding to smaller jumps of subnanometer size may reflect the generation of cracks. Al,03-TIC also exhibits a couple of pop-in marks at indentation loads higher than in the Ni-Zn ferrite. Sic exhibits no pop-in marks unlike the results reported by Page et al. [4] for singlecrystal Sic. Loading and unloading curves of indentation

at 0.2 mN in Sic repeat nearly the same curve indicating that the deformation at this load was mostly elastic. No pop-in marks in the loading curve of Sic are evident even at an indentation load of 15 mN. This suggests that there is probably no formation of cracks during indentation at these loads in Sic. During unloading and reloading, some hysteresis is observed in all bulk samples at higher loads. As expected, we note a significant difference in the load-displacement plots of the Sic coating and the bulk material. Hardness and elastic modulus profiles as functions of indentation depth for Ni-Zn ferrite, Al,O,TiC, and SIC are compared in Fig. 18 and Table 3. There are no significant variations observed in hardness and elastic modulus values as a function of indentation depth. Ni-Zn ferrite exhibits a lower hardness of about 12 GPa and elastic modulus of about 220 GPa as compared to A&O,-TiC and SIC. Bulk SIC exhibits a high hardness of about 35 GPa and elastic modulus of about 500 GPa. Comparison of hardness and elastic modulus values obtained by nanoindentation and by conventional techniques (Table 2) reveals that values obtained by nanoindentation are significantly higher.

B. Bhushan

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Fig. 22. SEM images of various regions and friction profile of a 500 pm long scratch made on Sic bulk at 2-25 mN. There is no significant damage or debris formation before 15 mN normal load. However, at about 24 mN normal load damage due to grain pull-out is visible in the image of region C, shown on the top of the friction profile.

,
i-

(/

.J__

.~_._ 4

~_._.. \ilrln*d

-____.._.--~L._

/II

1lUd.m-3

Fig. 20. SEM images of various regions and coefficient of friction profile of a 500 pm long scratch made on Ni-Zn ferrite bulk (a) at 2-25 mN. An abrupt increase in friction in (a) at about 10 mN is associated with damage to the surface. In some cases, grain pullout occurred at lower loads. An example is shown in (b) for a scratch made at 2-10 mN normal loads. Images of region B at 12 mN load in (a) and of region A at 3 mN in (b) clearly show grain pull-out during scratching.

Fig. 21. SEM images of various regions and friction profile of a 500 wrn long scratch made on Al,Os-TIC bulk at 2-25 mN. Ploughing into the surface is obvious right from the beginning of the scratch.

compared in Fig. 19. SEM images showing the damage events during a scratch, along with friction profiles, made at 2-25 mN normal load on these materials are shown in Figs. 20-22. Significant damage and generation of debris during scratching at 2-25 mN on Ni-Zn ferrite are visible after exceeding a normal load of 10 mN (Fig. 20(a)). The image of region B in Fig. 20(a) shows a tendency toward grain pull-out during scratching. We have also observed a grain pull-out damage even at a very low load of about 3 mN in a scratch made at 2-10 mN (Fig. 20(b)). The tendency for grain pull-out damage in Ni-Zn ferrite would result in premature failure and formation of large particles in the debris which are highly undesirable at the head-disk interface. In contrast to the Ni-Zn ferrite, Al,O,-TIC exhibits formation of debris right from the beginning of the scratch made at 2-25 mN load (Fig. 21). The amount of debris increased with increasing normal load. This is an unexpected observations, Al,O,-TiC should have higher scratch resistance because of its higher hardness (32 GPa) compared to that of Ni-Zn ferrite (14 GPa). Bulk Sic did not exhibit any signs of significant damage up to a normal load of about 15 mN (Fig. 22). However, when the normal load exceeded 15 mN some debris was formed and when the load approached about 24 mN some grain pull-out events were seen (see the image of region C in Fig. 22). Based on hardness, elastic modulus, and scratch resistance data, it is concluded that bulk Sic exhibits superior mechanical properties compared to Ni-Zn ferrite and A&O,-TiC bulk materials. 4. Conclusions Nanoindentation and microscratch studies reveal that an Sic coating followed by an a-C:H coating exhibit

3.2.2. Scratch resistance

Friction profiles of scratches made at 2-25 mN normal load on bulk Ni-Zn ferrite, Al,O,-Tic, and Sic are

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higher hardness, elastic modulus, and scratch resistance or adhesion compared with other coatings. Bulk Sic exhibits high hardness, elastic modulus, and scratch resistance compared to Ni-Zn ferrite and AI&-TiC bulk materials. Comparisons of microscratch data of bulk materials and coatings suggest that use of an Sic or a-C:H coating would result in a definite improvement in scratch resistance. The Sic coating exhibits a comparable coefficient of friction after run-in and lower wear than an a-C:H coating when slid against a sapphire ball. The Sic coating exhibits the best wear performance followed by a-C:H against a diamond tip as well as a sapphire ball compared to other coatings.

Status report: perpendicular contact recording 131 H. Hamilton, on rigid media,I. Magn. Sot. Jpn., 18 (Suppl. Sl) (1994) 171-178. The deformation ]41 T.F. Page, W.C. Oliver and C.J. McHargue, behavior of ceramic crystals subjected to very low load (nano)indentations, J. Mater. Res., 7 (1992) 450-473. behavior of silicon during na[51 G.M. Pharr, The anomalous noindentation, in Thin films: Stresses and Mechanical Properties III, Mater. Res. Sot. Symp. Proc., 239 (1992) 301-312. 161 B. Bhushan and B.K. Gupta, Handbook of Tribology: Materials, Coatings, and Surface Treatments, McGraw-Hill, New York, 1991. of silicon carbide and 171 R. Brutsch, Chemical vapor deposition its applications, Thin Solid Films, 126 (1985) 313-318. of the me]81 M.J. Loboda and M.K. Ferber, Characterization chanical properties of a-SiC:H films, J. Mater. Res., 8 (1993) 2908-2915. and Young s modulus ]91 N. Sawides and T.J. Bell, Microhardness of diamond and diamondlike carbon films, J. Appl. Phys., 72 (1992) 2791-2796. A.J. Kellock, N.-H. Cho and J.W. Ager III, [lOI B. Bhushan, Characterization of chemical bonding and physical characteristics of diamond-like amorphous carbon and diamond films, ): Mater. Res., 7 (1992) 404-410. D.K Veirs, M.D. Rubin, C.B. [HI N.-H. Cho, K.M. Krishnan, Hopper, B. Bhushan and D.B. Bogy, Chemical structure and physical properties of diamond-like amorphous carbon films prepared by magnetron sputtering, J. Mater. Res., 5 (1990) 2543-2554. ]I21 M. Rubin, C.B. Hopper, N.-H. Cho and B. Bhushan, Optical and mechanical properties of dc sputtered carbon films, /. Mater. Res., 5 (1990) 2538-2542. Role of mechanical properties ]I31 B. Bhushan and M.F.Doemer, and surface texture in the real area of contact of magnetic rigid disks, ASME J. Tribal., 111 (1989) 452-458. and G.W. Walker, Mechanical [I41 R.L. White, M.F. Doerner properties of carbon films for thin films disks, in Thin Fihns: Stresses and Mechanical properties II, Mater. Res. Sot. Symp. Proc., 188 (1990) 213-218. R. Jacobs, J. Smeets, J. Meneve, L. 1151 E.H.A. Dekempeneer, Eersels, B. Blanpain, J. Roos and D.J. Oostra, R.F. plasmaassisted chemical vapor deposition of diamond-like carbon: physical and mechanical properties, Thin Solid Films, 217 (1992) 56-61. and J. Chin, Structure and heat treatment ]I61 J.A. Thornton characteristics of sputter-deposited alumina, Ceram. Bull., 56 (1977) 504-508, 512. T.W. Wu, Microscratch and load relaxation tests for ultra-thin films, 1. Mater. Res., 6 (1991) 407-426. S.J. Bull, D.S. Rickerby, A. Matthews, A. Leyland, A.R. Pace and J. Valli, The use of scratch adhesion testing for the determination of interfacial adhesion: the importance of frictional drag, Surf. Coat. TechnoZ., 36 (1988) 503-517.

Acknowledgments We would like to thank Dr. Dimitre Latev of Censtor Corporation for providing the thin film samples used in this study. Bulk Ni-Zn ferrite and Al,O,TiC wafers were supplied by Storage Technology Corporation, Louisville, CO. Experimental Sic (Norton CRB-093) slider samples were supplied by Mr. Michael Boots of Prime Manufacturing Technology, San Diego, CA. We also thank John Mitchell of the Department of Geological Sciences for assistance in SEM imaging and Dr. Vilas Koinkar for AFM imaging. The research reported in this paper is part of an Ultra-High Density Recording Program funded by the National Storage Industry Consortium-Advanced Research Project Agency (Grant MDA 972-93-l-009) and the industrial membership of the Computer Microtribology and Contamination Laboratory.

References
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[2] B. Bhushan, Tribobgy and Mechanics of Magnetic Storage Devices, Springer, New York, 1990. H. Hamilton, R. Anderson and K. Goodson, Contact perpendicular recording on rigid media, IEEE Trans. Magn., 27 (1992) 49214926.