Dental Materials (2004) 20, 655662

www.intl.elsevierhealth.com/journals/dema

CAD/CAM-machining effects on Y-TZP zirconia

tera, Heike Rudolpha, Ralph G. Luthardta,*, Mandy S. Holzhu Volker Heroldb, Michael H. Waltera
a

Department of Prosthetic Dentistry, Dresden University of Technology, University Hospital Carl Gustav Carus, Dental School, Dresden, Germany b Technical Institute, Friedrich-Schiller-University, Jena, Germany
Received 1 August 2002; received in revised form 24 June 2003; accepted 12 August 2003

KEYWORDS
Advanced ceramics; YTZP; Zirconia; CAD/CAM; Surface analysis; Crowns; FPD; Grinding induced surface layer; Microcracks

Summary Objectives. Computer-Aided-Design/Computer-Aided-Manufacturing (CAD/CAM) techniques are gaining importance in fabricating crowns and xed partial dentures (FPDs) made of yttria stabilized tetragonal zirconia polycrystals (Y-TZP). The specic aims of this study were (1) to test the hypothesis that surface aws and microcracks are induced by the grinding of crowns (2) to analyze the material removal and the grinding-induced surface layer as well as to estimate the crack size caused by machining Y- TZP under conditions simulating the grinding of crowns. Methods. Y-TZP disks and sectioned cylinders with polished separation planes were used for the analysis of the grinding procedure. While simulating the inner surface grinding of crowns, feed and cutting depth were varied (vw 100; 75, 50 mm/min; ap 0:1; 0.06, 0.02 mm). SEM was used for the quantitative assessment of the machined surface. Results. While the crack length is not signicantly inuenced by the grinding parameters, the type of material removed varied with the cutting depth as well as with the feed. Grinding induced surface aws and microcracks were detected at the internal top surface of the crowns. Half-cylinders machined under conditions simulating the inner surface grinding of crowns showed crack lengths between 2 and 15 mm. Signicance. Sectioned specimens with polished section planes are suitable for the analysis of the grinding process using the face and peripheral grinding procedure. The inner surface grinding of xed restorations is the most challenging step of CAM of crowns and FPDs. Most important appeared to be the diamond tool, especially the number and shape of the active diamond grains. Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction
Inadequate mechanical long-term properties of conventional glass-ceramics limit their clinical application to inlays, veneers and single
*Corresponding author. Tel.: 49-351-4583572; fax: 49-3514585314. E-mail address: ralph.luthardt@mailbox.tu-dresden.de

crowns.1 5 The sintered, high alumina-content glass-inltrated ceramic core material (In-Ceramw Alumina) and the recently been developed lithium disilicate glass-ceramic (Empress 2w), respectively are recommended for anterior xed partial dentures (FPDs).6,7 and three-unit FPDs replacing the rst premolar.8 However, none of the current materials fulll the standards for posterior FPDs.6

0109-5641/$ - see front matter Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.dental.2003.08.007

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R.G. Luthardt et al. grinding parameter.24 Whereas the effects of zirconia and alumina due to the industrial grinding process with large diamond wheels is well known, factors inuencing the machining of Y-TZP for crowns and FPDs have not yet been examined. The specic aims of this study were: (1) to test the hypothesis that surface aws and microcracks are induced by the grinding of crowns (2) to analyze the material removed and the grinding-induced surface layer as well as to estimate the crack size caused by machining YTZP under conditions simulating the grinding of crowns. Therefore the grinding parameter had to be varied according to the parameter used during the CAM-process (cutting depth, feed).

This problem could be solved by the use of prefabricated advanced ceramics such as yttria stabilized tetragonal zirconia polycrystals (Y-TZP). In contrast to conventional dental ceramics Y-TZP is (1) composed of many very small particles (tetragonal crystallites metastable at room temperature , 0.5 mm,) without any glassy phase at the crystallite border and (2) distinguished by a crack initiation mechanism. In the stress eld of propagating cracks the matrix pressure on the tetragonal particles of Y-TZP is reduced by tensile stresses and a tetragonal (t) ! monoclinic (m) phase transformation occurs by a diffusionless shear process at near sonic velocities, similar to those of the martensite formation in quenched steel.9,10 The resulting volume expansion (3 5%) and the shear stresses formed in the particles affect martensitic transformation and pressure tensions on the matrix, opposing the opening of the crack and increasing the energy necessary for further crack growth.9,11,12 Due to these properties, as sintered Y-TZP showed a mean exural strength of 900 1000 MPa and a Weibull parameter m 10:7 to 14.9.10 Zirconia ceramics have been used in dentistry for orthodontic brackets 13 15 and post-core systems.16 20 Experimental studies showed, that copings of dense sintered Y-TZP could be machined using dental CAD/CAM-systems with improved stiffness of the grinding machine.21,22 However, copings of Y-TZP did not reach the increased fracture strength when compared with Procera Allceram copings, which could be expected due to the differences in the mechanical properties.22 The hypothesis proposed by the authors was that grinding-induced surface aws and microcracks are responsible for the limited fracture strength of Y-TZP copings. The inner surface grinding is characterized by the most challenging grinding conditions compared with the machining of the outer surface. Grinding of ceramics can act in two different directions: (1) on one hand residual surface compressive stresses were introduced that can increase the mean exural strength of zirconia toughened ceramics considerably, (2) on the other hand grinding introduces deep surface aws which act as stress concentrators and may become strength-determining if their length largely exceeds the depth of the grinding-induced surface compressive layer.10 The most important types of machining-induced near-surface characteristics are roughness, plastic deformation, damage and residual stresses.23 Abrasive machining comprises a mixture of brittle and ductile material removal.23 The strength-degradation problem can be reduced by grinding in the ductile mode using a suitable

Materials and methods

Sample preparation for the analysis of the crack size
Dense sintered Y-TZP ceramic cylinders (97 mol% ZrO2 , 3 mol% Y 2 O3 Metoxit AG, Thayngen, Switzerland; height and diameter 15 mm) were sectioned lengthwise using a diamond wheel (1A1R3001,25D126C75138AG, ALKU, Steinheim, Germany) mounted in a CNC surface grinder (Planomat 408, Blohm GmbH, Hamburg, Germany). The cylinders were cut, while a fully synthetic, water soluble grinding coolant free of mineral oil (DAW-AEROLAN VS, DAW Aerocit Schmierungstechnik GmbH, Werdau, Germany) was applied, using the feed velocity vf 20; 000 mm min21 ; the cutting depth ap 0:004 mm; and the spindle speed of n 2000 min21 : The sectioned surfaces were lapped (lapping wheel speed 40 min21, pressure 30 N cm22, diamond suspension D15) and polished (lapping wheel speed 40 min21, pressure 30 N cm22, diamond suspension D1). After highly accurate polishing of the sectioned surfaces, both parts of the half-cylinders stick to one another without any adhesive. The re-assembled cylinders were embedded in three-component cold mounting acrylic/polyester resin for embedding of materialographic specimens (Triox-2, Copenhagen, Denmark).

Sample preparation for the analysis of the surface nish

Dense sintered Y-TZP zirconia ceramic (97 mol% ZrO2, 3 mol% Y2O3, Metoxit AG, Thayngen, Switzerland) was used to produce specimens for the evaluation

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of the surface nish. Y-TZP zirconia ceramic disks (36 mm in diameter, 3 mm thick) were randomly divided into ten groups of four.

Table 1 Areas of the internal surfaces examined by SEM. Area Overview Crown margin (bulk) Crown margin (ne) Crown margin (surface) Internal wall Internal edge Top Magnication 20 100 , 1000 100 , 1000 100 , 1000 300 , 1000 50 , 1000 100 , 1000

Analysis of the inner surface grinding of crowns (preliminary investigations)

A Precident-DCSw milling-machine (DCS Production AG, Allschwil, Switzerland) was modied by installing a high frequency spindle with high stiffness (SC 53H, Precise GmbH, Leichlingen, Germany) xed on an advanced mounting device in order to improve the stiffness and to reduce vibration during grinding. The re-assembled cylinders were xed inside the holder of the Precident-DCSw milling machine orientated parallel to the XY -plane. The water-based oil emulsion grinding uid was used as a coolant. Cones and copings were machined using the procedure described elsewhere.21,22 After grinding, the re-assembled half-cylinders were manually taken apart again and cleaned (Fig. 1). Due to the sectioning of the cylinders and the polishing of the separation planes before grinding a view inside the machined ceramic uninuenced by further sample preparation processes such as cutting and polishing is possible. SEM-examination (Stereoscan 260, Cambridge Instruments, Cambridge, UK) was used in order to estimate the machined surfaces and to detect microcracks. Therefore, specied areas of the internal surfaces were examined with different magnication (Table 1).

Estimation of the crack size

Three re-assembled half-cylinders were used for the estimation of the crack size caused

Figure 1 Overview of one half-cylinder machined for a molar coping (a: machined inner surface; b: nonmachined outside; magnication 10-fold).

by simulated inner surface grinding of crowns. According to the results of the preliminary investigations, the machining of internal crown surfaces can be simulated well by face and peripheral grinding using the oscillating grinding method (Fig. 2). Face and peripheral grinding is dened by the parameter tools revolutions ns ; mesh ae ; feed vf and cutting depth ap : A software tool (DCS Production AG, Allschwil, Switzerland) was developed for the manufacturing of planes. From each re-assembled cylinder 0.3 mm in height were removed from the entire top surface with a feed vw 100 mm min21 and a cutting depth ap 0:1 mm: Afterwards two different procedures were applied to the top surfaces divided in three parallel zones orientated perpendicular to the section plane, not treating the middle zone. With a cutting depth ap 0:02 mm; 0.06 mm ceramic was removed at the rst zone of the top surface, while 0.3 mm was removed with a cutting depth ap 0:1 mm from the third zone of the top surface with a feed of 100, 75 and 50 mm/min, respectively. The diamond tool (1A1W-3-6: mixed grit sinter-diamond, top-surface at, DCS Production AG, Allschwil, Switzerland) used for the bulk material removal during inside and outside grinding of copings was chosen for this investigation. A spindle revolution of 60,000 min21 was applied. After surface treatment, the disks were cleaned manually with ethanol and sputtered with a gold layer of 20 40 nm (Cool-Sputter-Coater S150B, Edwards High Vacuum International, Crawley, England). SEM (XL 30 ESEM, Phillips) was used for quantitative assessment of the machined surface. Therefore, SEM-pictures were made with 30-, 100-, 1000- and 5000-fold magnication at the internal edge of the ground area. The depth of grinding induced surface aws and microcracks was measured perpendicular to the ground surface. The statistical signicance of the differences between the different grinding procedures regarding the direction of feed, the feed velocity vf and cutting depth ap were analyzed with one way analysis of variance (ANOVA, SPSS for

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Figure 2 Contact relation at face and peripheral grinding using the oscillating grinding method (ns tool revolutions, ae mesh, vf feed and ap cutting depth).

Windows Release 9.0, SPSS Software Corp., Munich, Germany).

Simulated inner surface grinding of crowns and surface nish

The modied Precident-DCS-Systemw and the software tool for the manufacturing of planes were used for the experiment. The disks were orientated horizontally and xed with colophonium on glass ceramic blocks that were mounted inside the holder of the Precident-DCS-Systemw in order to guarantee an orientation parallel to the XY -plane of the grinding machine. The top-surface at sinterdiamond tool described above was chosen for this experiment. The disks were reduced to 2.2 mm in thickness with the feed vf 100 mm min21 the cutting depth ap 0:1 the mesh ae 1 mm and the revolution of the spindle (60,000 min21). Afterwards the Y-TZP zirconia disks were ground to a thickness of 2.00 mm according to parameters indicated in Table 2. After surface treatment, the disks were cleaned manually with ethanol and sputtered with a gold layer of 20 to 40 nm (Sputter Coater). SEM (XL 30 ESEM, Phillips) was used for quantitative assessment of the machined surface. Three locations were randomly selected from each disk. SEM-pictures were made with 30-, 100-,
Table 2 Grinding parameter of the inner surface grinding of crowns. Series ns ae (mm) vf ap (mm) (mm min21) 0.1 0.1 0.1 0.06 0.06 0.06 0.02 0.02 0.02

1000- and 5000-fold magnication. The surface nish was categorized as: (1) material removed by plastic deformation, (2) mixed plastic/brittle material removed and (3) brittle material removed.

Results
The preliminary investigations dealing with the analysis of the inner surface grinding of crowns showed, that the nishing line as well as the internal wall showed only a thin grinding induced surface layer, while microcracking was detected at the internal top of the copings (Fig. 3).

Analysis of the crack size

The SEM images of the half-cylinders machined under conditions simulating the inner surface grinding of crowns showed similar effects. Grinding-induced surface aws (Fig. 4) as well as microcracks (Fig. 5) were detected. The mean depth of grinding induced surface aws and microcracks are shown in Table 3 for the measurements

1 2 3 4 5 6 7 8 9

100 75 50 Const. 60,000 Const. 1 100 75 50 100 75 50

Figure 3 Microcrack (arrow) at the internal top of the coping (a: non-machined outside; b: machined inner surface; magnication 1000-fold).

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Figure 4 Grinding related rim damage caused by grinding (a) magnication 300-fold (b) magnication 1000fold.

Figure 5 Grinding induced microcracks (a) magnication 100-fold (b) magnication 2000-fold.

Discussion
along l1 and against l2 the direction of rotation of the diamond tool. While no signicant differences were found for the grinding induced surface aws and microcracks dependent on the feed P 0:318 and cutting depth P 0:903; signicant differences were found for the direction of machining with regard to the direction of tool rotation P 0:000: According to the specic aims of this study, the experimental focus lay on surface aws and microcracks induced by the grinding process. Thus, parameters indicating an alteration of the internal structure of the bulk ceramic were analyzed. Consequently, values for surface roughness were not considered. The hypothesis that surface aws and microcracks are induced by the inner surface grinding of Y-TZP zirconia ceramic is conrmed. Analyzing
Table 3 Mean depth of grinding induced surface aws and microcracks for samples prepared with varied feed vf and cutting depth ap measured along l1 and against l2 the direction of rotation of the diamond tool. Series 1 2 3 7 8 9 vf (mm min21) 100 75 50 100 75 50 ap (mm) 0.1 0.1 0.1 0.02 0.02 0.02 l1 (mm) 3.05 2.55 1.89 2.03 1.86 1.47 l2 (mm) 6.84 7.38 14.97 6.175 14.85 11.45

Analysis of the surface nish

The SEM analysis of the Y-TZP zirconia ground with simulated inner-surface grinding showed three different types of surface nish, material removed by plastic deformation, mixed plastic/brittle material removed and brittle material removed, respectively (Fig. 6). Material removed by plastic deformation was detected with high cutting depth ae 0:1 mm with feed vf 100 and 75 mm min21, respectively while brittle material removal is increased with low cutting depth ae 0:02 mm (Table 4).

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Figure 6 Scanning electron micrographs of different types of material removal (a) plastic, (b) mixed plastic/brittle and (c) brittle, magnication 100-fold.

the grinding procedure of crowns, the grinding of the internal crown surface is most sophisticated due to the grinding and cooling process, which is usually limited by non-stationary front-end grinding conditions.21 These conditions could be simulated by face and peripheral grinding using the oscillating grinding method. The forces generated between the diamond tool and the ceramic workpiece during grinding are related to the machining condition as well as material properties.25 In accordance with clinical experience, the majority of failed crowns studied with quantitative fractography had shown initial cracks at the internal surface of the occlusal region where the greatest tensile stress concentrates and/or damage accumulates during clinical loading.26 30 Thus, the concentration of the grinding induced surface aws and microcracks located on the internal top surface should be minimized. On the one hand, grinding may introduce residual surface compressive stresses that can increase the strength of zirconia-toughened ceramics considerably while on the other hand, severe grinding may introduce deep surface aws, which

act as stress concentrators and become strength determining if their length largely exceeds the depth of the grinding induced surface compressive layer. The depth of the grinding induced surface aws and microcracks detected with the SEM

Table 4 Numbers of locations with different material removal dependent on the grinding parameters (total: 36). Series vf (mm min21) ap (mm) Plastic material removed Mixed plastic/ brittle material removed 3 2 3 1 2 2 3 1 1 Brittle material removed

1 2 3 4 5 6 7 8 9

100 75 50 100 75 50 100 75 50

0.1 0.1 0.1 0.06 0.06 0.06 0.02 0.02 0.02

1 1 0 0 0 0 0 0 0

0 1 1 3 2 2 1 3 3

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examination of crowns as well as by the simulated inner surface grinding should cause the limited strength of copings of Y-TZP zirconia compared with copings fabricated of alumina using the Procera technique. The material removed and the size of cracks induced while machining Y-TZP under conditions simulating the inner surface grinding of crowns is not dependent on the grinding parameters (cutting depth, feed). The surface of ground Y-TZP Zirconia is not inuenced by the machining parameter feed and cutting depth. Nevertheless, the direction of machining with regard to the direction of tool rotation is of signicant inuence. Overall, the kind of material removed showed an inhomogeneous distribution throughout the samples. Considering these ndings the major factor for the development of the grinding-induced surface layer and the microcracks appears to be the diamond tool. Since all parameters characterizing the grinding process were considered and constant in the experiment, the only possibly varying factor left has to be the diamond tool. The diamond tools used in the dental CAM process are small compared with those used in industrial applications. Therefore, the number of active grains is limited to less than 10. Consecutively, changes in the sharpness of the diamonds as well as the number of active grains which occur during the grinding process are of major importance for the ground surface properties.

References
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Conclusion
The results clearly indicate that grinding of densely sintered Y-TZP ceramics causes damage in the microstructure of the material. Varying the grinding parameter within a large range has not led to a solution for this problem. Therefore, alternative methods such as machining of partially sintered ceramics as well as non-grinding proling procedures should be developed in order to achieve CAD/CAM-fabricated crowns and FPDs of Y-TZP with improved strength and reliability.

Acknowledgements
This study was supported by the TMWFK (Thuringian Ministry of Science, Research and Culture), Grant B 403-97005 and in part by Girrbach Dental GmbH, Pforzheim, Germany.

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