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2008. CEO. dit par / Published by Elsevier Masson SAS. Tous droits rservs/All rights reserved

Performances tribologiques de lacier inoxydable, du TMA et du Cu-NiTi recouverts de DLC


Tribological performance of DLC-coated stainless steel, TMA and Cu-NiTi
Zakaria BENTAHAR1, Michel BARQUINS2, Martial CLIN3, Nezha BOUHAMMAD4, Khalid EL BOUSSIRI5

Rsum
Lamlioration de la friction et la rsistance lusure font partie des proprits des couches de carbone amorphe. Lobjectif de notre travail est dtudier les performances tribologiques des couches de carbone amorphe (DLC : Diamond-Like Carbon) dposes sur des fils orthodontiques : Cu-NiTi, acier et TMA. Les substrats tudis (acier inoxydable, TiMo, Cu-NiTi) sont des alliages frquemment utiliss en orthodontie. Des tiges .019 x .025 inch de 5 cm ont t fixes sur un support mtallique en acier inoxydable. Les dpts de DLC ont t raliss selon la technique plasma enhanced chemical vapor deposition. Un tribomtre muni dune balance, dun moteur et dun capteur lectronique a t utilis pour calculer le coefficient de frottement. Pour vrifier la reproductibilit, chaque test a t repris 10 fois. Lensemble des donnes a t recueilli laide du logiciel WinDataq Lite pour calculer le coefficient de frottement et reprsenter son volution en fonction du temps. Le coefficient de frottement du couple acier inoxydable recouvert de DLC/acier non recouvert a subi une augmentation par rapport au couple dacier non recouvert, alors que pour les deux autres couples (acier/Cu-NiTi et acier/TMA), le coefficient de frottement a diminu de 20 % 30 %.

Summary
Amorphous carbon films are characterized by lower friction and improved resistance to wear. The aim of our study was to investigate the tribological performance of diamond-like carbon (DLC) coated on CuNiTi, stainless steel and TMA orthodontic wires. The substrates investigated (CuNiTi, stainless steel and TiMo) are alloys frequently used in orthodontics. Five centimetre long .019x.025 rods were attached to a stainless steel support. DLC depositions were performed using the plasma-enhanced chemical vapor deposition technique. A tribometer fitted with scales, a motor and an electronic sensor were used to calculate the friction coefficient. To check reproducibility, each test was repeated 10 times. All the data were gathered using WinDataq Lite software in order to measure the friction coefficient and to show any changes occurring over time. The friction coefficient of the DLC-coated stainless steel vs DLCnon-coated stainless steel pair showed an increase as compared with the non-coated stainless steel pair. In contrast, the friction coefficient of the two other pairs (stainless steel/CuNiTi and stainless steel/TMA) decreased by 20 to 30%.

Mots-cls
DLC. Friction. Acier inoxydable. TMA. Cu-NiTi.
1

Key-words
DLC. Friction. Stainless steel. TMA. CuNiTi.

DCD, SQODF, Professeur agrg en orthodontie, Laboratoire de biomatriaux mtalliques, Facult de mdecine dentaire de Casablanca. 2 Professeur dhydrodynamique et mcanique physique, cole suprieure de physique chimie de la ville de Paris (ESPCI). 3 Professeur de physique, Laboratoire de physique de la matire condense, Facult des sciences dAmiens. 4 DCD, Pratique prive, Agadir, Maroc. 5 Professeur de biomatriaux, Docteur dtat en physico-chimie des matriaux, Laboratoire de biomatriaux mtalliques, Facult de mdecine dentaire de Casablanca.

Correspondance et tirs part / Correspondence and reprints: Z BENTAHAR, 3 rue Zemamra, Anfa, 20050 Casablanca, Maroc. zbentahar@wanadoo.net.ma

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Introduction
Lengouement actuel pour lutilisation des couches minces de carbone nanostructur dans le domaine biomdical est justifi par les proprits remarquables de ces matriaux : bonne biocompatibilit, inertie chimique, grande duret associes la capacit des couches limiter la diffusion des mtaux dans le sang et une excellente proprit lubrifiante [1-8]. En outre, des tests dusure ont rvl des ordres de grandeur similaires ceux des cramiques utilises dans le domaine des prothses mdicales. Cependant, les couches de carbone nanostructur prsentent un risque de dcohsion en raison des contraintes internes qui limitent leur application dans le domaine du traitement de surface des prothses mdicales. En odontologie, dautres applications des DLC semblent tre intressantes [9, 10]. En effet, le traitement orthodontique a recours, pour la correction des malpositions dentaires, des appareillages qui peuvent tre en mtal, en cramique ou en plastique. Le dplacement dentaire se fait par glissement de la dent sur un arc mtallique. La friction qui a lieu entre le verrou et larc fait partie des facteurs qui augmentent la dure du traitement. Pour faire face cette friction, lindustrie essaye de dvelopper des mtaux qui amliorent le glissement. Lamlioration de la friction et la rsistance lusure font partie des proprits des couches de carbone amorphe. Lobjectif de notre travail est dtudier les performances tribologiques des couches de carbone amorphe (DLC) dposes sur des fils orthodontiques en acier inoxydable, en Cu-NiTi et en TMA.

Introduction
The current popularity of thin films of nanostructured carbon used for biomedical purposes is based on the remarkable properties of these materials, namely, good biocompatibility, chemical inertia and extreme hardness combined with the ability of the coatings to limit the diffusion of the metals into the blood, as well as their excellent lubricating properties [1-8]. In addition, wear tests have revealed orders of magnitude similar to those of ceramics used for medical prostheses. However, nanostructured carbon films involve a risk of rupture on account of internal stresses, thus restricting their usage to the field of surface treatment of medical prostheses. In dental science, other DLC applications appear to offer benefits [9, 10]. Orthodontic treatment uses appliances which can be made of metal, ceramic or plastic in order to correct crooked teeth. Tooth displacement is generated by sliding the tooth along a metal archwire. The friction occurring between the brackets and the archwire is one of several factors responsible for increasing treatment duration. To counter this friction, industry is striving to develop metals which improve the sliding movement. Lower friction and enhanced resistance to wear are two of the characteristics of DLCs. The aim of this study is to investigate the tribological performance of DLCs deposited on stainless steel, CuNiTi and TMA orthodontic archwires.

Matriel et mthodes
Les substrats tudis (acier inoxydable, TMA, Cu-NiTi) sont des alliages frquemment utiliss en orthodontie. Des tiges .019 x .025 inch de 5 cm ont t fixes sur un support mtallique en acier inoxydable. Les dpts de couche de carbone ont t raliss au Laboratoire de physique de la matire condense de la Facult des sciences dAmiens (France). Le support contenant les tiges a t nettoy aux ultrasons en trois temps chacun de 16 mn. Le premier nettoyage a t ralis laide du trychlorothylne, suivi de lactone et, enfin, un dernier nettoyage lthanol. Les dpts de DLC ont t raliss selon la technique plasma enhanced chemical vapor deposition (fig. 1) [11]. Dans un premier temps, un etching a t ralis avec une pression de 3 Pa, une puissance de 250 W et une nergie de -770 V. Les couches de carbone amorphe ont t dposes selon les paramtres suivants : 1 Pa, 250 W, -454 V pendant 95 min. Un tribomtre muni dune balance rgle en quilibre, dun moteur et dun capteur lectronique a t utilis pour les tests de frottement et pour raliser les tests dusure. Lalimentation du moteur tait assure laide dun gnrateur branch un stabilisateur de courant. Sur le moteur tait connecte une carte dacquisition numrique DATAQ DI-194RS branche sur un

Material and methods


The substrates studied (stainless steel, TMA, CuNiTi) are alloys frequently used in orthodontics. Five-centimeter long .019x.025 rods were attached to a stainless steel support. The DLC depositing was performed at the Laboratory of condensed matter physics at the Faculty of Science in Amiens, France. The support holding the rods was cleaned by ultrasound in three 16 minutes stages. The first cleaning was done using trichloroethylene, the second with acetone and the last with ethanol. The DLC depositing was performed using the plasma enhanced chemical vapor deposition technique (fig. 1) [11]. Firstly, etching was performed at 3 Pa pressure, 250 W power and -77V energy. The DLC was deposited using the following parameters: 1Pa; 250W, -454V for 95min.

A tribometer fitted with scales set at balance, a motor and an electronic sensor was used for the friction tests and to perform the wear tests. The motor was powered by a generator hooked up to a current stabilizer. To the motor we connected a DATAQ DI-194RS digital data acquisition card plugged into a computer. A hygrometer and a thermometer were placed in the work space in

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Tribological performance of DLC-coated stainless steel, TMA and Cu-NiTi

Fig. 1 : Sputtering.
Fig. 1: Sputtering.

Fig. 2 : volution du coefficient de frottement du couple acier/acier non recouvert.


Fig. 2: Changes in the friction coefficient of the non-coated stainless steel/stainless steel pair.

ordinateur. Un hygromtre et un thermomtre, dposs dans le champ de travail, ont t utiliss pour calculer lhygromtrie et la temprature. Les fils en tige taient fixs sur les porte-chantillons du moteur et de la balance. Avant chaque manipulation, les chantillons non recouverts de DLC taient nettoys lactone. Plusieurs couples de frottement forms de tiges recouvertes et non recouvertes de DLC ont t tests. Lacier inoxydable non recouvert de carbone composait toujours une surface du couple. La force normale choisie tait de 10 g et le moteur tournait une vitesse de 684 m/s. Des tests dtalonnage ont t raliss avant et la fin de chaque manipulation. Lvolution du coefficient de frottement en fonction du temps a t enregistre. Pour vrifier la reproductibilit, chaque test a t repris 10 fois. Enfin, un test dusure a t ralis pour chaque couple.

order to measure hygrometry and temperature. The rods were attached to the specimen-holders on the motor and scales.

Prior to each pass, the non-DLC-coated samples were cleaned with acetone. Several friction pairs including DLC-coated and non-DLC-coated rods were then tested. One surface in the pair always consisted of a non-carbon-coated stainless steel rod. The usual force chosen was 10 gr and the motor operated at a speed of 684 m/s. Calibration tests were performed before and after each pass. Changes in the friction coefficient over time were recorded. In order to check reproducibility, each test was performed 10 times. Lastly, a wear test was performed on each pair.

Rsultats
Pour le couple form par des tiges en acier inoxydable non recouvert par du carbone amorphe, le coefficient de frottement a suivi une volution rgulire tout au long du trajet (fig. 2). Le coefficient de frottement statique (s) dpendant de la force ncessaire pour amorcer le glissement est situ 0,13 et le coefficient de frottement dynamique (d) est situ le long du trajet 0,07. Le recouvrement de la surface par du DLC a modifi le comportement tribologique (fig. 3). Le coefficient de frottement statique (s) est pass de 0,13 0,42. Deux zones irrgulires ont apparu, au dbut du mouvement et entre 13 et 16 secondes. Le coefficient de frottement dynamique (d) est situ 0,14. Aprs 107 passages (fig. 4), nous avons assist une accentuation de la dtrioration de la surface matrialise par une trajectoire accidente. Le coefficient de frottement dynamique a chang de valeur trois reprises entre 0,28 et 0,36.

Results
Regarding the pair of non-DLC-coated stainless steel rods, the friction coefficient changed steadily throughout the trajectory (fig. 2). The static friction coefficient (s) reflecting the force required to commence the sliding movement was 0.13 and the dynamic friction coefficient (d) along the length of the trajectory was 0.07. Coating the surface with DLC modified the tribological behaviour (fig. 3). The static friction coefficient (s) increased from 0.13 to 0.42. Two irregular areas were observed at the onset of the movement and between 13 and 16 seconds. The dynamic friction coefficient (d) was 0.14. After 107 passes (fig. 4), we witnessed a deterioration of the surface as evidenced by jerky movements. The dynamic friction coefficient changed value three times between 0.28 and 0.36.

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Fig. 3 : volution du coefficient de frottement du couple acier/acier recouvert de DLC.


Fig. 3: Changes in the friction coefficient of the DLC-coated stainless steel/stainless steel pair.

Fig. 4 : volution du coefficient de frottement du couple acier/acier recouvert de DLC aprs un test dusure.
Fig. 4: Changes in the friction coefficient of the DLC-coated stainless steel/stainless steel pair after wear test.

Le glissement dune tige en acier sur une tige en Cu-NiTi non recouverte de DLC a montr des valeurs du coefficient de frottement suprieur au couple prcdent. Le coefficient statique (s) est situ 0,37 et le coefficient dynamique (d) se situe 0,24 (fig. 5). La trajectoire tait plus ou moins rgulire avec des pics de petite taille. Le recouvrement de la surface du Cu-NiTi par du DLC a amlior le coefficient de frottement dynamique puisquil a t presque divis de moiti, passant de 0,24 0,14 entre 2 et 7 secondes (fig. 6). Une zone irrgulire est apparue entre 7 secondes et 23 secondes. Dans cet intervalle de temps, le coefficient a subi une augmentation jusqu 0,28 puis une diminution pour reprendre sa valeur initiale 0,14. Aprs 96 passages, linterface a subi une dtrioration avec une augmentation du coefficient du frottement 0,33 (fig. 7). La mme amlioration a t obtenue avec le couple acier/ Cu-NiTi et le couple acier/TMA. Sans recouvrement, le coefficient de frottement statique ( s) a t de 0,24 et le coefficient dynamique ( d) est situ environ 0,20. La trajectoire de variation est presque linaire, except lintervalle de temps entre 16 et 23 secondes o nous avons eu deux valeurs minimales 16 et 22 secondes (fig. 8). Le recouvrement de la tige TMA par DLC a diminu les coefficients de frottement statique ( s) et dynamique (d) puisquils sont passs respectivement de 0,24 0,14 et de 0,20 0,18 (fig. 9). Lendommagement de linterface aprs 61 passages est bien matrialis par une augmentation du coefficient de frottement pour atteindre une valeur de 0,34 (fig. 10).

A stainless steel rod sliding along a non-DLC-coated rod provided friction coefficient values higher than those of the previous pair. The static coefficient (s) was 0.37 and the dynamic coefficient (d) 0.24 (fig. 5). The trajectory was more or less even with only minor peaks. Coating the surface of CuNiTi with DLC improved the dynamic friction coefficient which almost halved from 0.24 to 0.14 between 2 and 7 seconds (fig. 6). An irregular zone was observed between 7 and 23 seconds. During this interval, the coefficient increased to 0.28 before returning to its initial value of 0.14. After 96 passes, the interface deteriorated and the friction coefficient increased to 0.33 (fig. 7).

Similar improvement was achieved with the stainless steel/ CuNiTi and the stainless steel TMA pairs. Uncoated, the static friction coefficient (s) was 0.24 and the dynamic coefficient (d) was approximately 0.20. The variation trajectory was almost linear apart from the interval between 16 and 23 seconds when we observed two minimum values at 16 and at 22 seconds (fig. 8). Coating the TMA rod with DLC reduced the static friction (s) and dynamic friction (d) coefficients as they decreased, respectively, from 0.24 to 0.14 and from 0.20 to 0.18 (fig. 9). The damage to the interface after 61 passes was evidenced by the increase in the friction coefficient which increased to 0.34 (fig. 10).

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Tribological performance of DLC-coated stainless steel, TMA and Cu-NiTi

Fig. 5 : volution du coefficient de frottement du couple acier/CuNiTi non recouvert.


Fig. 5: Changes in the friction coefficient of the uncoated stainless steel/CuNiTi pair.

Fig. 6 : volution du coefficient de frottement du couple acier/CuNiTi recouvert de DLC.


Fig. 6: Changes in the friction coefficient of the DLC-coated stainless steel/CuNiTi pair.

Fig. 7 : volution du coefficient de frottement du couple acier/CuNiTi recouvert de DLC aprs un test dusure.
Fig. 7: Changes in the friction coefficient of the DLC-coated stainless steel/CuNiTi pair after wear test.

Fig. 8 : volution du coefficient de frottement du couple acier/TMA non recouvert.


Fig. 8: Changes in the friction coefficient of the uncoated stainless steel/ TMA pair.

Discussion
Les alliages acier, Cu-NiTi et TMA recouverts par des couches DLC hydrognes dposes par la technique de Plasma Enhanced Chemical Vapor Deposition et testes dans lair ambiant avec une humidit contrle ont montr un comportement tribologique variable dun couple lautre. Conformment aux rsultats obtenus dans dautres tudes sintressant aux films DLC, le recouvrement des alliages Cu-NiTi et TMA a permis davoir une amlioration importante de leur comportement tribologique.

Discussion
Stainless steel, CuNiTi and TMA alloys coated with hydrogenated DLC using the Plasma Enhanced Chemical Vapor Deposition technique and tested in ambient air in controled humidity demonstrated variations of tribological behavior between the different pairs. The results agreed with those obtained in other studies related to DLC coating and showed that coating CuNiTi and TMA alloys with DLC provided enhanced tribological behavior.

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Fig. 9 : volution du coefficient de frottement du couple acier/TMA recouvert de DLC.


Fig. 9: Changes in the friction coefficient of the DLC-coated stainless steel/TMA pair.s

Fig. 10 : volution du coefficient de frottement du couple acier/TMA recouvert de DLC aprs un test dusure.
Fig. 10: Changes in the friction coefficient of the DLC-coated stainless steel/TMA pair after wear test.

Le recouvrement des tiges en Cu-NiTi a permis de rduire, de presque la moiti, le coefficient de frottement. Cette rduction importante peut sexpliquer par les proprits lubrifiantes des couches DLC. Lintervalle de temps compris entre 7 et 23 secondes est marqu par une augmentation du coefficient de frottement pour atteindre le double de sa valeur initiale suivie dune diminution (fig. 8). Laugmentation du coefficient de frottement dynamique (d) peut tre explique par une dtrioration de la couche DLC au niveau de certains endroits mettant ainsi en contact direct les surfaces des deux composants du couple. Aprs cette augmentation, le coefficient a diminu pour revenir de nouveau sa valeur initiale. Sachant quune diminution du coefficient de friction implique la prsence dun lubrifiant, on peut dire que cette baisse indique quun mcanisme dautolubrification sest produit. Il peut bien sagir de la graphitisation de surface [12-17]. Ce processus impliquant la libration dhydrogne au niveau de la surface [18] va permettre une rduction de la friction grce une rserve constante de matriel sous forme de graphite obtenue partir dune transformation structurale de phases Sp3 en Sp2 intressant les produits dusure [17]. Paralllement la graphitisation, on peut galement supposer la formation dun film de transfert au niveau de la contreface rsultant de la compaction dune partie des dbris dusure transfre partir de la surface DLC [19, 20]. Ce film assure la protection de la contreface contre lusure et rend plus efficace le mcanisme dautolubrification [12-15, 17]. Aprs 96 passages, le coefficient de frottement est pass 0,33. Cette augmentation peut tre due lusure tendue et llimination dune partie de la couche DLC. Aprs recouvrement par DLC, on a not, sur le couple acier/ TMA, une amlioration des coefficients de frottement mettant en

Coating CuNiTi rods reduced the friction coefficient by almost half. This major reduction can be accounted for by the lubricating properties of the DLC film. The time interval between 7 and 23 seconds was marked by an increased friction coefficient which reached twice the initial value followed by a fall (fig. 8). The increased dynamic friction coefficient (d) was probably due to the deterioration of the DLC film at certain points, thus bringing into direct contact the surface of the two components forming the pair. Following this increase, the coefficient decreased, returning to its initial value. Given that a drop in the friction coefficient implies the presence of a lubricant, it can be surmised that this decrease points to the presence of a selflubricating mechanism which might involve surface graphitization [12-17].

This process involves the release of hydrogen at the surface [18] which triggers a reduced rate of friction because of the constant presence of a pool of graphite material resulting from the structural transformation of Sp3 phases into Sp2 and involving the material produced by wear and tear [17]. In addition to the graphitization process, one can assume that a transfer film formed on the opposing surface as a result of compaction of some of the wear debris transferred from the DLC surface [19, 20]. This film ensures the protection of the opposing surface against wear and enhances the auto-lubrication process [12-15, 17]. Following 96 passes, the friction coefficient increased to 0.33, possibly as a result of prolonged wear and tear and to the elimination of some of the DLC film. Following coating with DLC, we observed, on the stainless steel/ TMA pair, an improvement in the friction coefficients, thus demons-

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Tribological performance of DLC-coated stainless steel, TMA and Cu-NiTi

vidence le rle lubrifiant des couches DLC. La figure 9 montre une lgre augmentation progressive avec le temps du coefficient de frottement sans pour autant dpasser 0,20. Cette augmentation peut avoir comme cause un dtachement du film DLC. Probablement, ladhsion des couches DLC sur TMA ntait pas bonne et suffisante pour pouvoir rsister aux contraintes. Lamlioration de ladhsion DLC/TMA doit tre aussi recherche dans les futures tudes afin de mieux claircir le comportement tribologique de ces alliages recouverts par DLC. Plusieurs approches ont t dcrites [21-27]. Lobjectif commun est doptimiser ladhsion de DLC sur son substrat. Aprs 61 passages, le coefficient de frottement a augment 0,26 marquant une limination dune partie du DLC. Pour le couple acier/acier, contrairement ce qui a t rapport par dautres tudes, le coefficient de frottement aprs recouvrement par DLC a subi une augmentation. Or, il est important de souligner que les proprits tribologiques des DLC dpendent troitement des paramtres de dpt et de ceux de lenvironnement o elles sont testes [17, 18, 20, 22, 28-32]. Deux films dposs par la mme technique et sur un mme alliage peuvent avoir des comportements tribologiques diffrents. Il est donc possible que les paramtres utiliss dans notre tude ne fussent pas optimaux pour obtenir une couche idale permettant damliorer le glissement du couple form par les tiges en acier.

trating the lubricating role played by the DLC film. Figure 9 displays a slight gradual increase over time of the friction coefficient although never exceeding 0.20. This increase may be due to flaking of the DLC coating. It is likely that the adherence of the DLC on the TMA was inadequate to withstand stress. In future studies, means of improving DLC/TMA adherence should be sought in order to shed light on the tribological behaviour of these DLCcoated alloys. Several approaches have already been described [21-27]. Their common goal was to optimize DLC adherence on the substrate. After 61 passes, the friction coefficient rose to 0.26, thus pointing to the elimination of some of the DLC film.

As regards the stainless steel/stainless steel pairing, and in contrast with findings reported in other studies, the friction coefficient increased after coating with DLC. It is important then to emphasize that the tribological properties of DLC are highly dependent upon the parameters governing the coating process as well as the setting in which they are tested [17, 18, 20, 22, 28-32]. Two films deposited using the same technique on the same alloy can have different tribological behaviors. It is possible, therefore, that the parameters used in our study were not optimal to obtain an ideal film allowing an improvement of the sliding properties of the pair of stainless steel rods.

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