Abstract Service life of machine parts used in the oil and gas industry can be expanded by using coatings that improve surface properties such as wear and corrosion resistance. DLC coatings are known for their low friction coefficient, high wear resistance and chemical inertness. TiSiCN films are hard ceramics, so they provide good resistance to abrasive and erosive wear. In this work, these two coatings deposited on alloy steel AISI 4140 are comparatively analyzed. Thickness was measured and the coatings were characterized by XPS, DRX and Raman spectroscopy. Pin-on-disk adhesive wear and abrasive wear tests (ASTM G65) were carried out. Adhesion was evaluated by scratch test. Corrosion resistance was evaluated by salt spray test and potentiodynamic tests. DLC coatings presented low friction coefficient μ ~ 0,2, and a volume loss twice as low as TiSiCN, whereas the latter presented 30 times the abrasive wear resistance. The adhesion of TiSiCN was also superior. DLC showed higher corrosion resistance.

RESUMEN La vida en servicio de elementos de máquinas utilizados en la industria del gas y del petróleo puede ser extendida con el uso de recubrimientos que permiten mejorar las propiedades superficiales, como la resistencia al desgaste y a la corrosión. Los recubrimientos DLC son conocidos por su bajo coeficiente de fricción, alta resistencia al desgaste e inercia química. Las películas del tipo TiSiCN son cerámicas duras, por lo que otorgan una buena resistencia al desgaste abrasivo y erosivo. En este trabajo se analizan de forma comparativa estos dos recubrimientos cuando son depositados sobre un acero de media aleación AISI 4140. Se midió espesor y se hizo caracterización por XPS, DRX y espectroscopía Raman. Se realizaron ensayos de desgaste adhesivo tipo Pin-on-Disk y desgaste abrasivo (ASTM G65). Se evaluó la adhesión por Scrach Test. La resistencia a la corrosión se evaluó mediante cámara de niebla salina y ensayos potenciodinámicos. El DLC presentó un bajo coeficiente de fricción μ ~ 0,2, con una pérdida de volumen dos veces menor que el TiSiCN, mientras que este último presentó una resistencia al desgaste abrasivo 30 veces superior. La adhesión del TiSiCN también fue superior. El DLC mostró una mayor resistencia a la corrosión.

In this work the influence of pre-treatment cleaning processes in the adhesion of TiN films deposited by the plasma based ion implantation and deposition (PBII&D) process over plasma nitrided AISI 316L stainless steel was investigated, varying the gas composition, the duration of the sputtering process and the temperature in the same deposition chamber. The TiN film morphology was scrutinized with scanning electron microscopy on the surface complemented with focus ion beam for the cross section. The film microstructure was characterized with X ray diffraction. The adhesion of the coatings was studied using the Scratch Test with constant load at different values and the Rockwell C indentation method as well. It was found that only with the sputtering carried out in a H2 - Ar gas mixing at 300 ºC temperature used as pre-treatment was successful to prepare the nitrided surface for the subsequent TiN deposition by the PBII&D process.

ABSTRACT Hydrogenated carbon-based films, such as DLC (“Diamond Like Carbon”), have interesting properties such as excellent tribological behavior, low friction coefficient, high superficial hardness and good wear resistance; they are chemically inert and highly corrosion resistant. They are deposited by means of PACVD (plasma-assisted chemical vapor deposition) with variable film thickness. The load carrying capacity grows with the thickness, so it is possible to deposit thick films on “soft” steels (e.g. low alloyed steels). When increasing coating thickness, surface defects are generated during the deposition process compromising their excellent properties. In this work, different metal substrates have been used to compare adhesion and quantify superficial defects: AISI 316L, DIN 42CrMo4 (AISI 4140) and Böhler K110 (AISI D2). The films were deposited at different temperatures, changing the silicon content and the coating thickness. The samples were placed in the furnace on different positions (standing, lying or up-side down). The films were analyzed with optical and electron microscopy, 3D topography profilometer, and they were tested under sliding wear conditions. Friction coefficient and wear volume were measured, with an average friction coefficient which resulted below 0.05. A higher amount of surface defects was obtained on lying samples compared to the ones up-side down. The quantity of defects increased with the thickness of the coating and decreased with the temperature. The geometry and the growth mechanism of the defects were analyzed.

ABSTRACT Martensitic stainless steels can be used in different applications such as surgical instruments where a good wear and corrosion resistance are required. Surface modification treatments such as nitriding improve the mechanical properties of these steels, however; they affect the corrosion resistance. For this reason, the DLC (Diamond Like Carbon) coatings deposition can be convenient. The wear and corrosion behaviour was studied in duplex samples (nitrided and PACVD coated) and they were compared with nitrided and only coated samples and with those without treatment, only heat treated (quench and tempering). The coatings were analyzed by Raman spectroscopy and EDS. Pin on disk tests were performed and the adhesion was evaluated using Scratch Test and Rockwell C Indentation. The nanohardness was measured with a Berkovich indenter. The corrosion tests for surgical instruments (according to the Standard ASTM F 1089 -02) and Spray Salt Fog tests were carried out. In the DLC coatings, the ID/IG ratio was 0.8 and the hydrogen content was calculated and resulted to be about 20 %. The coating thickness was 2 µm and the hardness reached 24 GPa. The nitrided layer thickness was 10 µm. The duplex and coated samples presented low friction coefficient and the wear volume loss was undetectable. The coatings had good corrosion behaviour in the corrosion tests. Nevertheless, the nitrided sample presented a corroded region in the copper sulfate and boil tests. The duplex samples had better adhesion than the coated samples in scratch test and indentation Rockwell C.

RESUMEN Los aceros inoxidables martensíticos como el AISI 420 tienen múltiples aplicaciones, entre ellas instrumentos quirúrgicos, donde se requiere buena resistencia al desgaste y a la corrosión. Los tratamientos de modificación superficial, como la nitruración iónica, permiten mejorar las propiedades mecánicas de estos aceros pero afectan su resistencia a la corrosión. Por esta razón, un tratamiento posterior de deposición de recubrimiento tipo DLC (“Diamond Like Carbon”, carbono símil diamante) puede ser conveniente. En este trabajo se estudió el comportamiento al desgaste y a la corrosión de muestras dúplex (nitruradas y recubiertas por PACVD) y se compararon con muestras nitruradas, sólo recubiertas, nitruradas y sólo templadas y revenidas. Se analizaron los recubrimientos con espectroscopia Raman y EDS. Se realizaron ensayos de desgaste tipo “pin on disk” y se evaluó la adhesión mediante ensayos de Scratch Test e indentación Rockwell C. Se midió nanodureza con indentador Berkovich. Se llevaron a cabo los ensayos propuestos para instrumentos quirúrgicos en la Norma F 1089-02 (prueba de agua hirviendo y de hisopado con sulfato de cobre) y ensayos de niebla salina. Estos recubrimientos tienen una relación ID/IG de 0,8 y bajo contenido de hidrógeno aproximadamente del 20 %. El espesor de los recubrimientos fue de 2 µm y la dureza alcanzó 24 GPa. La capa nitrurada tuvo un espesor de 10 µm. Las muestras dúplex y recubierta presentaron bajo coeficiente de fricción y el volumen desgastado fue indetectable. Además, tuvieron buen comportamiento a la corrosión en el ensayo de niebla salina y en los ensayos propuestos en la Norma ASTM F 1089-02. No obstante, la muestra sólo nitrurada presentó una región corroída en el ensayo de sulfato de cobre y en el de agua hirviendo. La muestra dúplex presentó mejor adhesión que la muestra sólo recubierta en los ensayos de Scratch Test y de indentación Rockwell C.