Littérature scientifique sur le sujet « Arc-DLC coating »

Hard coatings are increasingly being used in medicine to protect metal endoprostheses The experimental process for the high-productive synthesis of high-quality diamond-like carbon (DLC) coatings with high hardness and a sufficiently high level of adhesion to the spherical shaped parts of the hip joint made from the stainless steel or cobalt-chrome alloy have been developed. DLC coating deposition was performed by vacuum-arc method from a high-productive source of the filtered vacuum-arc carbon plasma of rectilinear type with a "magnetic island". The high degree of thickness uniformity in the coating on the head of the hip joint with a high adhesion to the metal joint base was developed. Modernization of the vacuum arc plasma source allowed to accelerate the cathode spot motion, exclude substrate overheating and increase the diamond-like carbon hardness up to 30-40 GPa. The high adhesion level was achieved as a result of the high voltage pulsed of substrate bias potential use and multilayer architecture of DLC coating. The DLC coating on the heads of hip endoprosthesis did not peel off when boiling endoprosthesis or when immersing it into the liquid nitrogen. JEL O31

Abstract Hard coatings are increasingly being used in medicine to protect metal endoprostheses The experimental process for the high-productive synthesis of high-quality diamond-like carbon (DLC) coatings with high hardness and a sufficiently high level of adhesion to the spherical shaped parts of the hip joint made from the stainless steel or cobalt-chrome alloy have been developed. DLC coating deposition was performed by vacuum-arc method from a high-productive source of the filtered vacuum-arc carbon plasma of rectilinear type with a "magnetic island". The high degree of thickness uniformity in the coating on the head of the hip joint with a high adhesion to the metal joint base was developed. Modernization of the vacuum arc plasma source allowed to accelerate the cathode spot motion, exclude substrate overheating and increase the diamond-like carbon hardness up to 30-40 GPa. The high adhesion level was achieved as a result of the high voltage pulsed of substrate bias potential use and multilayer architecture of DLC coating. The DLC coating on the heads of hip endoprosthesis did not peel off when boiling endoprosthesis or when immersing it into the liquid nitrogen.

The aim of this study is to investigate the wear resistance of diamond-like carbon (DLC) films and wear debris of polyethylene using pin-on-disc testing on two groups of CoCrMo discs with DLC coatings. DLC coatings deposited with use high productive vacuum-arc filtered plasma source in two regimes: with and without Ti interlayer on CoCrMo discs. The Orthopaedic Innovation Centre performed 2.5 million cycles (Mc) of POD testing on two groups of CoCrMo discs with DLC based on ASTM G99-17. The discs used were made of wrought low carbon alloy CoCrMo according to ASTM F1537. Wear performance of the PE pins against the DLC coated discs was determined and reported below. Lubricant samples were collected for each group after 0.5 and 2.5 Mc of testing, and used to characterize wear particles. All PE pins were assessed for damage features following 2.5 Mc of wear testing. The damage features identified included burnishing, scratching and grooving. The new process of DLC coating deposition from filtered vacuum arc plasma flows allows obtaining the stable DLC coating on the CoCrMo substrate. Thus, considering the low friction coefficient and the stable behavior of DLC such coating would be highly perspective for CoCrMo artificial joint implants.

Diamond-like carbon (DLC) and TiN coatings were deposited on the 304 austenitic stainless steel(SUS304) substrates by using unbalanced magnetron sputtering and arc ion plating techniques, respectively. The phase structure and surface morphology of coatings were characterized by SEM and XRD.The electrochemical corrosion of two coatings in different electrochemical solutions (including3.5%NaCl,10%HCl,20%NaOH) were investigated by electrochemical workstation.The result showed that DLC coating was amorphous structure and TiN coating was nano-crystalline structure.The surface of DLC coating was smooth and dense,while TiN coating existed pits.In 10%HCl and 3.5%NaCl solutions,the corrosion resistance of DLC coating increased by 4.16 and 10.9 times compared with SUS304 and increased by 5.16 and 1.11 times compared with TiN coating,respectively.But in 20%NaOH solution, the corrosion resistance of DLC was not superior to SUS304 and TiN coating.In 10%HCl solution,the corrosion resistance of TiN coating increased by 9.81 times compared with 304 SUS304.But in 3.5%NaCl and 20%NaOH solutions,the corrosion resistance of TiN coating was worse than SUS304.

Microarc oxidation (MAO) treatment produces a thick Al2O3 coating on the 15SiCp/2024 aluminum matrix composite. After pretreatment of Ti ion implantation, a thin diamond-like carbon film (DLC) was deposited on the top of polished Al2O3 coating by a pulsed filtered cathodic vacuum arc (FCVA) deposition system with a metal vapor vacuum arc (MEVVA) source. The morphology and tribological properties of the duplex Al2O3 /DLC multiplayer coating were investigated by Raman spectroscopy, scanning electron microscopy (SEM) and SRV ball-on-disk friction tester. It is found that the duplex Al2O3 /DLC coating had good adhesion and a low friction coefficient of less than 0.07. As compared to a single Al2O3 or DLC coating, the duplex Al2O3 /DLC coating on aluminum matrix composite exhibited a better wear resistance against ZrO2 ball under dry sliding, because the Al2O3 coating as an intermediate layer improved load support for the top DLC coating on 15SiCp/2024 composite substrate, meanwhile the top DLC coating displayed low friction coefficient.

The combinations of TiAl-doped DLC and TiAlN/TiN layers were designed to deposit on the tool steels using cathodic arc evaporation in a continuously single batch process. The economic advantage in depositing the combined coating in one production scale of PVD system is of practical importance. The TiAl-doped DLC as lubricant coatings were synthesized by using arc plasma sources mounted with Ti50Al50-target to emit high energy ion plasma to activate the decomposition of acetylene reactive gases. The results show that the TiAl-doped DLC and TiAlN/TiN combined coatings retained lower friction coefficient at approximately 0.15 during the steady-state sliding. The lubricity and wear resistance of TiAl-doped DLC/TiAlN/TiN coatings is then demonstrated to potentially be applied to the cutting tools with no lubricants.

In this work, the diamond-like carbon and titanium nitride (DLC/TiN) multilayer coatings were prepared on a cemented tungsten carbide substrate (WC—3 wt.% Co) using the cathodic vacuum arc physical vapor deposition (Arc-PVD) method and pulsed Arc-PVD method with a graphite cathode for the deposition of TiN and carbon layers, respectively. The structural and mechanical properties of the prepared coatings were studied, and different techniques, such as scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, and microindentation techniques investigated their microstructure, composition, and phases. The prepared coatings had a multilayer structure with distinct phases of DLC, TiN, and carbide substrate. The potentiodynamic polarization method (PDP) was performed for the DLC/TiN multilayer coatings in 3% NaCl solution to evaluate the corrosion resistance of the prepared coatings. It has been shown that the DLC layer provided the coating with a polarization resistance of 564.46 kΩ. Moreover, it has been demonstrated that the DLC/TiN coatings had a high hardness of 38.7–40.4 GPa, which can help to extend the wood-cutting tools’ life.

Purpose The disbonding of DLC coating is a main failure mode in the high-speed cavitation condition, which shortens the service life of the bearing. This study aims to investigate influence of adhesion strength on cavitation erosion resistance of DLC coating. Design/methodology/approach Three DLC coatings with different adhesion strengths were grown on the 304 steel surfaces by using a cathodic arc plasma deposition method. Cavitation tests were performed by using a vibratory test rig to investigate the influence of adhesion strength on cavitation erosion resistance of a DLC coating. The cavitation mechanism of the substrate-coating systems was further discussed by means of surface analyses. Findings The results indicated that, the residual stress decreased and then increased with the increasing DLC coating thickness from 1 µm to 2.9 µm, and the lower residual stress can improve the adhesion strength of the DLC coating to the substrate. It was also concluded that, the plastic deformation as well as the fracture occurred on the DLC coating surface at the same time, owing to higher residual stress and poorer adhesion strength. However, lower residual stress and better adhesion strength could help resist the occurrence of the coating fracture. Originality/value Cavitation tests were performed by using a vibratory test rig to investigate the influence of adhesion strength on cavitation erosion resistance of the DLC coating. The plastic deformation and the fracture occurred on the DLC coating surface at the same time, owing to higher residual stress and poorer adhesion of coating. Lower residual stress and better adhesion of coating could resist the occurrence of the DLC coating fracture.

The purpose of the study was to ascertain the corrosion resistance in Hanks’ solution of Cr-Ni-Mo stainless steel (AISI 316L) coated with diamond-like carbon (DLC) coatings to establish its suitability for biomedical applications, e.g., as temporary implants. The influence of the carbon coating thickness as well as the correlated effect of the metallic sublayer type and defects present in DLC films on corrosion propagation were discussed. The results obtained were compared with findings on the adhesion of DLC to the steel substrate. The synthesis of carbon thin films with Cr and Ti adhesive sublayers was performed using a combined DC and a high-power-impulse vacuum-arc process. Evaluation of the corrosion resistance was carried out by means of potentiodynamic polarisation tests and scanning electron microscopy. Adhesive properties of the sublayer/DLC coating systems were measured using a scratch tester. It was found that systems with Ti sublayers were less susceptible to the corrosion processes, particularly to pitting. The best anti-corrosion properties were obtained by merging Ti with a DLC coating with a thickness equal to 0.5 μm. The protective properties of the Cr/DLC systems were independent of the carbon coating thickness. On the other hand, the DLC coatings with the Cr sublayer showed better adhesion to the substrate.

In order to improve the lower adhesion strength of Si-DLC coatings to the substrate and enhance its wear resistance, Si-DLC coatings with different transition layers (AlTiSiN, AlCrN and AlTiCrN) were prepared on 304 austenitic stainless steel substrates using multi-arc ion plating technique. The effects of different transition layers on the properties of Si-DLC were characterized by scanning electron microscopy, X-ray diffractometer, nanoindentation, confocal microscopy, Rockwell hardness tester, Raman test and wear test to find the optimal Si-DLC transition layer. The results show that the Si-DLC coating with AlTiSiN as the transition layer has an ID/IG of 0.71, the highest hardness of 26.7 Gpa, low surface roughness, the highest compressive stress, the best bond strength and the best wear resistance.

Les objectifs de cette thèse de doctorat étaient de caractériser l’efficacité des revêtements de surface développé pour lutter contre les problèmes de transfert de matière rencontrés lors de la mise en forme de l’aluminium à chaud, et d'étudier ces mécanismes de transfert. Le matériau utilisé était un alliage d'aluminium AA 6082-T6, largement employé dans la fabrication de composants automobiles.Le test de Compression-Translation à chaud (WHUST) a été retenu comme tribomètre principal pour cette étude. Afin de contrôler précisément les températures des essais, un dispositif miniaturisé du WHUST a été conçu afin être intégré dans la chambre chauffante de la plateforme Bruker UMT TriboLab. Les tests préliminaires avec ce nouvel appareil ont montré un empilement significatif de matière devant le contacteur. De nouvelles équations analytiques ont donc été développées pour identifier le coefficient de frottement de Coulomb (COF) et le facteur de frottement (loi de Tresca) en tenant compte de cet empilement de matière.Le WHUST a ensuite été utilisé pour évaluer les performances tribologiques de trois revêtements PVD commerciaux : un AlCrN, un TiAlN et un Arc-DLC. Les expériences ont été menées sans lubrifiant, à des températures variant de 300 °C à 500 °C, sous des pressions de contact comprises entre 40 et 100 MPa, avec une vitesse de glissement égale à 0,5 mm/s. Les résultats ont montré que le revêtement Arc-DLC était plus efficace que les revêtements AlCrN et TiAlN pour atténuer les problèmes de transfert d’aluminium. En particulier, le revêtement Arc-DLC provoquait moins d'adhésion et moins de transfert d'aluminium, notamment lors du début du glissement. Ces résultats ont été confirmés par des essais sous des pressions de contact plus élevées, réalisés à l’aide l’essai de forgeage en T à chaud (HVGCT).Dans la deuxième partie de cette thèse, le revêtement Arc-DLC a été sélectionné pour étudier en détail les mécanismes de transfert d’aluminium sur les outils de mise en forme. Des essais ont été réalisés avec une courte distance de glissement (2 mm) pour examiner les premières étapes du transfert d’aluminium, tandis que des tests avec une distance de glissement de 38 mm ont permis d’étudier l’évolution du transfert. Les expériences ont été conduites aux mêmes températures d’essai (300-500°C), avec deux vitesses de glissement différentes, 0,5 mm/s et 5,0 mm/s, et toujours sans lubrifiant. Les topographies de surface et les images SEM prises le long de la piste de frottement ont montré que le transfert d'aluminium se produit en deux étapes principales : une phase initiale principalement due au labourage mécanique, suivie d'une phase de croissance dominée, en fonction des températures et des vitesses de glissement, par du labourage mécanique ou par de l'adhésion.Dans la dernière partie de cette thèse, l'apprentissage automatique (ML) a été utilisé pour étudier les mécanismes de transfert d’aluminium. Les topographies de surface et les images SEM prises le long de la piste de frottement ont été analysées. Elles ont été classifiées à l’aide de cinq algorithmes d’apprentissage automatique simples et d'une architecture de réseau neuronal convolutif (CNN) personnalisée. Il a été démontré que le ML appliqué aux données topographiques et le CNN appliqué aux images SEM permettaient tous deux d’identifier les modes d’usure avec précision
The aims of this PhD thesis were to find effective surface coatings to prevent the material transfer issue and to study the mechanisms of material transfer in the hot forming of aluminum alloy. The workpiece material was AA 6082-T6 aluminum alloy, which is widely used to produce automotive components.The warm and hot upsetting sliding test (WHUST) was selected as the main tribometer in this study. To control the testing temperatures precisely, a scaled-down apparatus of the WHUST was designed to integrate into the heating chamber of the Bruker UMT TriboLab platform. The preliminary experiments of the new apparatus found that the pile-up material significantly occurred in front of the contactor due to the high friction at the interface and the deformation characteristic of the aluminum alloy at high temperatures. From this point, the pile-up material was considered as a new parameter in analytical equations used to identify the Coulomb coefficient of friction (COF) and the shear friction factor.The new apparatus of the WHUST was then used to evaluate the tribological performance of three commercial PVD coatings: AlCrN, TiAlN, and Arc-DLC. The experiments were performed at temperatures between 300˚C and 500˚C, at 0.5 mm/s of sliding speed under non-lubrication contact conditions. Those conditions led to the mean contact pressure between 40 MPa and 100 MPa. The results showed that the Arc-DLC coating had better efficiency in alleviating the aluminum transfer issue than the AlCrN and TiAlN coatings. The Arc-DLC coating caused less adhesive to the aluminum alloy and less transferred aluminum, especially in the initial period. Moreover, these findings were consolidated under higher contact pressure by using the hot V-groove compression test (HVGCT).Following that, the Arc-DLC coating was selected to study the mechanisms of aluminum transfer on the forming tool in detail. The WHUST was performed with the specific short sliding distance (2 mm) to investigate the initial stage of aluminum transfer, while the full sliding distance (38 mm) was used to examine the evolution of aluminum transfer. The experiments were conducted at the same testing temperatures with two different sliding speeds, 0.5 mm/s and 5.0 mm/s, under non-lubrication contact conditions. It was found that the aluminum transfer in the initial stage was mainly caused by mechanical plowing. Then, during the grow-up stage, the aluminum transfer was dominated by mechanical plowing and/or adhesive bonding, depending on the testing temperatures and the sliding velocities. Additionally, the different transfer mechanisms caused dissimilar COFs, surface characteristics along the friction track of the specimen, as well as transferred aluminum.In the last part of this PhD thesis, Machine Learning (ML) was involved to study the mechanisms of aluminum transfer. The previous part found that the wear characteristics along the friction track could be a significant indicator to differentiate the transfer mechanisms. Thus, the surface topographies and the SEM images along the friction track were used to classify by five simple ML algorithms and a custom Convolutional Neural Network (CNN) architecture, respectively. It was proved that the ML with topographic data and the CNN with SEM image data had the potential to identify the wear mode accurately

Die vorliegende Dissertation behandelt Charakterisierung, Modellbildung sowie Anwendung einer magnetfeldgestützten Hohlkathoden-Bogenentladung. Hohlkathoden sind seit den 1960er Jahren Gegenstand grundlagen- sowie anwendungsorientierter Forschung und werden seit 20 Jahren am Fraunhofer-Institut für Elektronenstrahl- und Plasmatechnik für die Anwendung auf dem Gebiet der Vakuumbeschichtung weiterentwickelt. Ziel dieser Arbeit ist es, die technologischen Fortschritte physikalisch zu verstehen und gezielte Weiterentwicklungen für spezifische Einsatzgebiete zu ermöglichen. In der untersuchten Hohlkathodenbauform ist das aus Tantal bestehende, vom Arbeitsgas Argon durchströmte Kathodenröhrchen koaxial von einer Ringanode sowie von einer Magnetfeldspule umgeben. Die Entladung wird durch Hochspannungspulse gezündet, worauf sich ein diffuser Bogen im Röhrchen (internes Plasma) ausbildet. Das Röhrchen wird von Plasmaionen auf hohe Temperaturen geheizt, die eine thermionische Emission von Elektronen ermöglichen, welche das Plasma speisen. Das technologisch nutzbare externe Plasma wird im Vakuumrezipienten durch Wechselwirkung der Gasteilchen mit Strahlelektronen aus der Kathode erzeugt. Bei starker Reduktion des Arbeitsgasflusses wird die Entladung durch das Magnetfeld der Spule stabilisiert. Der experimentelle Befund, dass dadurch Plasmadichte und -reichweite sowie ggf. die Ladungsträgerenergien im Rezipienten aufgrund des intensiveren Elektronenstrahls wesentlich gesteigert werden können, wird durch ortsaufgelöste Langmuir-Sondenmessung, optische Emissionsspektroskopie und energieaufgelöste Massenspektrometrie ausführlich belegt und nach der Lösung von Strom- und Wärmebilanzgleichungen durch die Verhältnisse im Kathodenröhrchen begründet. Neben Argon werden auch typische Reaktivgase der Vakuumbeschichtung im Hohlkathodenplasma betrachtet: zum einen Stickstoff und Sauerstoff, die in reaktiven PVD-Prozessen (physikalische Dampfphasenabscheidung) zur Beschichtung mit Oxid- bzw. Nitridschichten zum Einsatz kommen und durch Ionisation, Dissoziation und Anregung im Hohlkathodenplasma verbesserte Schichteigenschaften ermöglichen; zum anderen Azetylen, das bei PECVD (plasmagestützte chemische Dampfphasenabscheidung) von amorphen wasserstoffhaltigen Kohlenstoffschichten z. B. für tribologische oder biokompatible Beschichtungen genutzt wird. Azetylen wird durch Streuprozesse mit Elektronen und Ionen im Plasma aufgespalten, wodurch schichtbildende Spezies erzeugt werden, die am Substrat kondensieren. Durch die Wahl der Plasmaparameter sowie durch abgestimmte Substratbiasspannung und Substratkühlung lassen sich die Beschichtungsrate einstellen sowie polymer-, graphit- oder diamantartige Eigenschaften erzielen. Neben der Plasmadiagnostik mittels energieaufgelöster Massenspektrometrie werden die erzeugten Kohlenstoffschichten vorgestellt und hinsichtlich Härte, Zusammensetzung und Morphologie analysiert
In the present thesis, characterization, modeling and application of a magnetically enhanced hollow cathode arc discharge are presented. Since the 1960s, hollow cathodes are being studied in basic and applied research. At Fraunhofer Institute for Electron Beam and Plasma Technology, further development concerning the application in vacuum coating technology has been carried out for about twenty years. The present work targets on physically understanding the technological progress in order to enable specific further development and application. In the investigated hollow cathode device, a ring-shaped anode and a magnetic field coil are arranged coaxially around the tantalum cathode tube, which is flown through by argon as the working gas. The discharge is ignited by high voltage pulses establishing a diffuse arc within the cathode tube (internal plasma). The cathode is being heated by the plasma ions to high temperatures, which leads to thermionic emission of electrons sustaining the plasma. The external plasma in the vacuum chamber, which can be used for technological applications, is generated by collisions of gas atoms with beam electrons originating from the cathode. In the case of strongly reduced working gas flow, the discharge is stabilized by the magnetic field of the coil; the related experimental findings such as significantly increased plasma density and range as well as higher charge carrier energies in the external plasma are extensively proved by spatially resolved Langmuir probe measurements, optical emission spectroscopy, and energy-resolved ion mass spectrometry. Furthermore, the results are correlated to the conditions within the cathode tube by solving the current and heat balance equations. Besides argon, typical reactive gases used in vacuum coating are examined in the hollow cathode plasma, too. First, nitrogen and oxygen, which are applied in PVD (physical vapor deposition) processes for the deposition of oxide and nitride layers, are ionized, dissociated, and excited by plasma processes. In the case of practical application, this plasma activation leads to improved film properties. Second, acetylene is used as a precursor for PECVD (plasma-enhanced chemical vapor deposition) of amorphous hydrogenated carbon films, e.g. for tribological or biocompatible applications. Acetylene is cracked by electron and ion scattering in the plasma providing film-forming species to be deposited on the substrate. The deposition rate as well as the polymeric, graphitic, or diamond-like properties can be controlled by plasma parameters, a defined substrate bias, and substrate cooling. The hollow cathode-generated acetylene plasma has been characterized by energy-resolved ion mass spectrometry, and the carbon films obtained are analyzed regarding hardness, film composition, and morphology

Die vorliegende Dissertation behandelt Charakterisierung, Modellbildung sowie Anwendung einer magnetfeldgestützten Hohlkathoden-Bogenentladung. Hohlkathoden sind seit den 1960er Jahren Gegenstand grundlagen- sowie anwendungsorientierter Forschung und werden seit 20 Jahren am Fraunhofer-Institut für Elektronenstrahl- und Plasmatechnik für die Anwendung auf dem Gebiet der Vakuumbeschichtung weiterentwickelt. Ziel dieser Arbeit ist es, die technologischen Fortschritte physikalisch zu verstehen und gezielte Weiterentwicklungen für spezifische Einsatzgebiete zu ermöglichen. In der untersuchten Hohlkathodenbauform ist das aus Tantal bestehende, vom Arbeitsgas Argon durchströmte Kathodenröhrchen koaxial von einer Ringanode sowie von einer Magnetfeldspule umgeben. Die Entladung wird durch Hochspannungspulse gezündet, worauf sich ein diffuser Bogen im Röhrchen (internes Plasma) ausbildet. Das Röhrchen wird von Plasmaionen auf hohe Temperaturen geheizt, die eine thermionische Emission von Elektronen ermöglichen, welche das Plasma speisen. Das technologisch nutzbare externe Plasma wird im Vakuumrezipienten durch Wechselwirkung der Gasteilchen mit Strahlelektronen aus der Kathode erzeugt. Bei starker Reduktion des Arbeitsgasflusses wird die Entladung durch das Magnetfeld der Spule stabilisiert. Der experimentelle Befund, dass dadurch Plasmadichte und -reichweite sowie ggf. die Ladungsträgerenergien im Rezipienten aufgrund des intensiveren Elektronenstrahls wesentlich gesteigert werden können, wird durch ortsaufgelöste Langmuir-Sondenmessung, optische Emissionsspektroskopie und energieaufgelöste Massenspektrometrie ausführlich belegt und nach der Lösung von Strom- und Wärmebilanzgleichungen durch die Verhältnisse im Kathodenröhrchen begründet. Neben Argon werden auch typische Reaktivgase der Vakuumbeschichtung im Hohlkathodenplasma betrachtet: zum einen Stickstoff und Sauerstoff, die in reaktiven PVD-Prozessen (physikalische Dampfphasenabscheidung) zur Beschichtung mit Oxid- bzw. Nitridschichten zum Einsatz kommen und durch Ionisation, Dissoziation und Anregung im Hohlkathodenplasma verbesserte Schichteigenschaften ermöglichen; zum anderen Azetylen, das bei PECVD (plasmagestützte chemische Dampfphasenabscheidung) von amorphen wasserstoffhaltigen Kohlenstoffschichten z. B. für tribologische oder biokompatible Beschichtungen genutzt wird. Azetylen wird durch Streuprozesse mit Elektronen und Ionen im Plasma aufgespalten, wodurch schichtbildende Spezies erzeugt werden, die am Substrat kondensieren. Durch die Wahl der Plasmaparameter sowie durch abgestimmte Substratbiasspannung und Substratkühlung lassen sich die Beschichtungsrate einstellen sowie polymer-, graphit- oder diamantartige Eigenschaften erzielen. Neben der Plasmadiagnostik mittels energieaufgelöster Massenspektrometrie werden die erzeugten Kohlenstoffschichten vorgestellt und hinsichtlich Härte, Zusammensetzung und Morphologie analysiert.
In the present thesis, characterization, modeling and application of a magnetically enhanced hollow cathode arc discharge are presented. Since the 1960s, hollow cathodes are being studied in basic and applied research. At Fraunhofer Institute for Electron Beam and Plasma Technology, further development concerning the application in vacuum coating technology has been carried out for about twenty years. The present work targets on physically understanding the technological progress in order to enable specific further development and application. In the investigated hollow cathode device, a ring-shaped anode and a magnetic field coil are arranged coaxially around the tantalum cathode tube, which is flown through by argon as the working gas. The discharge is ignited by high voltage pulses establishing a diffuse arc within the cathode tube (internal plasma). The cathode is being heated by the plasma ions to high temperatures, which leads to thermionic emission of electrons sustaining the plasma. The external plasma in the vacuum chamber, which can be used for technological applications, is generated by collisions of gas atoms with beam electrons originating from the cathode. In the case of strongly reduced working gas flow, the discharge is stabilized by the magnetic field of the coil; the related experimental findings such as significantly increased plasma density and range as well as higher charge carrier energies in the external plasma are extensively proved by spatially resolved Langmuir probe measurements, optical emission spectroscopy, and energy-resolved ion mass spectrometry. Furthermore, the results are correlated to the conditions within the cathode tube by solving the current and heat balance equations. Besides argon, typical reactive gases used in vacuum coating are examined in the hollow cathode plasma, too. First, nitrogen and oxygen, which are applied in PVD (physical vapor deposition) processes for the deposition of oxide and nitride layers, are ionized, dissociated, and excited by plasma processes. In the case of practical application, this plasma activation leads to improved film properties. Second, acetylene is used as a precursor for PECVD (plasma-enhanced chemical vapor deposition) of amorphous hydrogenated carbon films, e.g. for tribological or biocompatible applications. Acetylene is cracked by electron and ion scattering in the plasma providing film-forming species to be deposited on the substrate. The deposition rate as well as the polymeric, graphitic, or diamond-like properties can be controlled by plasma parameters, a defined substrate bias, and substrate cooling. The hollow cathode-generated acetylene plasma has been characterized by energy-resolved ion mass spectrometry, and the carbon films obtained are analyzed regarding hardness, film composition, and morphology.

碩士
明道管理學院
材料暨系統工程研究所
93
Abstract In this work, the combinations of metal-doped DLC and TiAlN/TiN double-layered films were designed to deposit on the tool steels using cathodic arc evaporation in a single process. The economic advantage in depositing the combined coating in one production scale PVD coating system is of practical importance. The TiAl-doped DLC as lubricant coatings were synthesized with TiAl-target arc sources to emit ion plasma to activate acetylene reactive gases. Experiments were carried out to deposit TiAl-DLC on TiAlN/TiN/M2 tool steel for different substrate bias ranging from -50 to -200 V, hydrocarbon gases (C2H2) pressure 10 to 25 mtorr and temperature fixed at 180 ℃. Scanning electron microscopy (SEM), Auger electron spectroscopy (AES), micro-Raman spectroscopy. X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) techniques were employed to analysis the microstructure properties of TiAl-doped DLC coatings. Vicker's and tribometer tester were used to measure the mechanical properties of TiAl-doped DLC coatings. The results indicated that the bias voltage and hydrocarbon gases (C2H2) pressure plays a major role in the microstructure change in the deposition of TiAl-doped DLC films. The profile ID/IG and sp3/sp2 ratio corresponds to the change of microhardness profile as the bias voltage or the hydrocarbon gases (C2H2) pressure varied. And, TiAl metals are in the form of small nanocrystallites of pure metal or metal carbides dispersed throughout the carbon network. The tribo-analysis indicated that the coatings exhibited steady-state friction in the range of 0.15 - 0.25 to the end of 2 km travel distance. Interesting optimum wear rate corresponded to the steady-state low coefficient of friction of DLC films due to formation of graphitized layer. The lubricity and wear resistance of TiAl-doped DLC coatings is then demonstrated to potentially be applied to the cutting tools with no lubricants. To summary, the optimum condition and properties of TiAl-doped DLC coatings was appeared at the bias of-120 V and the hydrocarbon gases (C2H2) pressure of 15 mtorr.

For biomedical application in the field of artificial hip joints diamond-like carbon (DLC) coatings have been widely studied due to their excellent mechanical, tribological and biological properties. The wear particles as the main factor limiting the life expectancy of hip joints have attracted more and more interest, not only the number of them, but also the distribution of their size. In this study we have deposited DLC coatings on stainless steel (P2000) by a vacuum arc adjustable from anodic to cathodic operation mode. To improve the adhesion of the DLC coating on P2000, titanium as a metallic interlayer was deposited by cathodic vacuum arc evaporation. The frequency distribution of wear particles generated using a disc-on-disc test was measured by a particle size analyzer. It was shown that the maximum of the frequency distribution e.g. at —1000 V bias can be shifted to below 1 µm with increasing anode/cathode diameter ratio da/dc.

Abstract Diamond-like carbon (DLC) films have excellent properties such as high hardness, low friction coefficient, high wear resistance, chemical inertness and so on. Because DLC film is considered as an effective coating material to improve their surface properties, this films are used in various applications such as parts for automobiles engines, hard disk surfaces, cutting tools and dies, and so on. DLC films consist of a mixture of sp2 bonded carbon atoms and sp3 bonded carbon atoms. Among them, ta-C film is known as the hardest and strongest film since it mainly consists of sp3 bonded carbon atoms. One of deposition methods to form ta-C is Filtered Cathodic Vacuum Arc (FCVA). The characteristic of this method is that it is possible to remove the droplets and form a high-quality film.. However, even though lots of mechanical components which require ta-C coating have three-dimensionally shapes, it is difficult to coat ta-C film three dimensionally by using FCVA process. At present, researches on 3D deposition of amorphous carbon films on three dimensional components is still insufficient, and investigation reports on the deposition mechanism and characterization of the deposited films are even more limited. In this study, we tried to deposit films on 3D components by the FCVA method and evaluated the microstructure and surface morphologies of films. Although films were coated successfully in the entire surfaces, different properties were showed depending on the location of components. These properties were investigated by Raman spectroscopy and laser microscope.

Abstract Diamond like-carbon (DLC) coatings is a form of amorphous consisting of sp2-bonded and sp3-bonded phase. Among the DLC series, DLC coatings containing a large percentage of sp3 ratio, referred as tetrahedral amorphous carbon (ta-C) coatings, have attracted significant attention as protective coatings in various fields such as tribological applications and automobile components that demand superior durability, chemical inertness and low friction at high temperature. Particularly, the filtered cathodic vacuum arc (FCVA) technique with an energetic plasma can deposit the ta-C coating, but it has a drawback such as decreasing deposition rate and occurring macroparticles. Research on morphological and structural change of defects in ta-C coatings fabricated by FCVA is important for understanding their wear and friction behavior. In this study, the types of defects presented on a ta-C coating were classified as spike, droplet and pore with their morphology, structural and mechanical properties. The tribological behavior of the coating was characterized by ball-on-disk test using a Si3N4 ball at a testing temperature of 170 °C. In order to confirm the effect of defects in the ta-C coating on the tribological behavior, the defects in a designated area were investigated as a function of different sliding cycles. Initially, a running-in cycle is maintained until 2,000 cycles, following which a steady-state value of 0.1 is observed from sliding cycles of 2,000 to 10,000. At the end of 10,000 cycles, the wear rate of the ta-C coating is 4.3 × 10−6 mm3/Nm. Structural changes among the defects are apparent on droplet and pore after the friction test at 170 °C. The nodular defects including spikes and droplet is grinded off on top surface of that and is retained until 1,000 cycles. In steady state up to 6,000 cycles, droplet was survived, on the other hand, the spikes are almost polished from sliding.