Micro deep drawing of micro cups by using DLC film coated blank holders and dies

Lubrication is one of the key problems in metal forming, and this is even more important in micro forming because of size effect on friction. Diamond like carbon (DLC) film coated blank holders and dies were used in forming micro cups with drawing blank diameters of 2 mm. A plasma immersion ion implantation and deposition (PIIID) process was proposed to treat the blank holders and drawing dies. Raman spectrum, scratch test, and ball-on-disc test were used to investigate the structure, adhesion strength, and tribological property of the DLC films. The micro deep drawing experiments were carried out at room temperature on a universal testing machine at a drawing velocity of 0.1 mm/s without lubrication, and under the lubrication of castor oil and DLC film. The results showed that the micro cups were well formed with a minimum inner diameter of 0.95 mm under the lubrication of DLC film. The DLC film which dramatically decreased the drawing force and increased the limit drawing ratio (LDR) was better than other lubrication conditions and can be chosen as a proper lubricant in micro forming for mass production.     

Large-area uniform hydrogen-free diamond-like carbon films prepared by unbalanced magnetron sputtering for infrared anti-reflection coatings

The hydrogen-free diamond-like carbon (DLC) films are potential materials to be used as infrared anti-reflection protective coatings if their optical absorption can be reduced to get relatively thick films needed. In this study, hydrogen-free DLC films were deposited by the physical vapor deposition (PVD) method in an unbalanced magnetron sputtering (UBMS) system with a rectangle graphite target of 440 × 80 mm in the argon atmosphere. The UBMS system was described in detail and the magnetron field distribution of the target was denoted in this work. The film thickness uniformity was investigated and the results showed that this system is capable of depositing uniform films larger than 150 mm in diameter. The infrared transmission spectra of DLC films were analyzed by a FTIR spectrometer, the results indicating that transparent films were obtained in the infrared region for the single side DLC coated on the silicon and germanium substrates, and about 68.83% and 63.05% transmittance were achieved respectively at the wave number of 2983 /cm, close to theoretical value for non-absorption carbon material. No obvious absorption peaks were found between 5000 and 800 /cm. The refractive index and extinction coefficient of the DLC films deposited under optimized conditions were about 2.08 and 0.067 respectively at the wavelength of 1600 nm. These important optical characteristics showed that the hydrogen-free DLC films prepared in the UBMS system were suitable for infrared transmission enhancement applications.     

A study of hard diamond-like carbon films in mid-frequency dual-magnetron sputtering

A series of hydrogen-free diamond-like carbon (DLC) films were deposited by a mid-frequency dual-magnetron sputtering under basic conditions of Cr and C target power density between 6 and 18 W/cm², bias voltage in a range of − 100 V to − 200 V, and a pure argon atmosphere. Microstructure, microhardness, adhesion, friction and wear properties were investigated for the DLC films to be used as protective films on cutting tools and forming dies, etc. The DLC films exhibited some combined superior properties: high hardness of 30–46 GPa, good adhesion of critical load of 50–65 N, and friction coefficient about 0.1 in air condition. Properties of the magnetron-sputtered carbon films showed a strong dependence on flux and energy of ion bombardment during growth of the films.     

Coating of DLC film by pulsed discharge plasma CVD

Diamond-like carbon (DLC) films were deposited onto Ti plate substrate by means of pulsed discharge (PD) plasma chemical vapor deposition (CVD) from gas mixture of methane and hydrogen, and their structures were investigated with transmission electron microscope (TEM). When the polarity of the substrate was negative, the DLC film was grown on the substrate. The transmission electron diffraction (TED) pattern of the deposited film, which was shaved with knife from the surface of the substrate, showed that both TiC and diamond structures were formed, showing that the DLC film can be coated with good adhesion by means of the formation of TiC interlayer. The coatings of DLC films onto a stainless steel plate and a drill of WC, on which Ti film were deposited previously, was also succeeded by the PD plasma CVD method with good adhesion.     

Fabrication of DLC thin films with improved diamond-like carbon character by the application of external magnetic field

Diamond-like carbon (DLC) thin films were grown on Si-(100) substrates by a magnetically-assisted pulsed laser deposition (PLD) technique. The role of magnetic field on the structural, morphological, mechanical properties and deposition rate of DLC thin films has been studied. The obtained films were characterized by Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), field emission scanning electron microscopy (FE-SEM) and nanoindentation techniques. It was found that the diamond-like character, thickness and deposition rate of the DLC films increase in the presence of magnetic field. The films deposited under magnetic field exhibit a denser microstructure and smoother surface with lower surface roughness. Meanwhile, the mechanical properties of the magnetically processed DLC thin films experience an improvement, relative to the conventionally processed ones. It seems that the DLC films deposited under magnetic field can be better candidate for hard and wear resistance coating applications.     

Structural effects of nanocomposite films of amorphous carbon and metal deposited by pulsed-DC reactive magnetron sputtering

The relationship between metal-induced (W, Mo, Nb and Ti) structures and the surface properties of Me–DLC thin films is discussed. Nanocomposite films were deposited on c–Si wafers by pulsed-DC reactive magnetron sputtering controlling the gas ratio CH₄/Ar. The sputtering process of metals such as Ti, Nb and Mo (unlike the tungsten) in the presence of methane shows a low reactivity at low methane concentration. The deposition rate and the spatial distribution of sputtered material depend of Z-ratio of each metal. The surface contamination of metal targets by carbon, owing to methane dilution, limits the incorporation of metals into DLC films according to an exponential decay. Results of electron probe microanalysis and X-ray photoelectron spectroscopy indicate a C rich Me/C composition ratio for low relative methane flows. According to the depth profile by secondary ion mass spectrometry, the films are systematically homogeneous in depth, whereas at high carbon contents they exhibit a metal-rich interfacial layer on the substrate. Moreover, high resolution transmission electron microscopy has evidenced important structural modifications with respect to DLC standard films, with marked differences for each Me/C combination, providing nanodendritic, nanocrystallized or multilayered structures. These particular nanostructures favour the stress decrease and induce significant changes in the tribological characteristics of the films. This study shows the possibilities of controlling the amorphous carbon films structure and surface properties by introducing metal in the DLC matrix.     

Electrochemical characteristics of lithium metal anodes with diamond like carbon film coating layer

To overcome the poor electrochemical characteristics of lithium metal anodes due to the dendrite formations, diamond like carbon (DLC) films were deposited onto the surface of lithium metal by radio frequency-plasma enhanced chemical vapor deposition (CVD) technique using acetylene gas as carbon precursor. The substrate temperature was selected as the main experimental parameter to control the bonding characteristic (sp²/sp³ ratio) of the films. The presence of diamond like structures was confirmed by Raman and Fourier transform infra red spectroscopy. The DLC coated lithium metal was then characterized as an anode material for lithium secondary batteries. The results showed that the DLC coated lithium metal anodes exhibited better electrochemical characteristics in terms of higher specific capacity and smaller interfacial impedance. These improved characteristics were attributed to the presence of DLC film coating which might suppress the dendrite's formation by protecting the lithium metal surface from the direct contact with the electrolyte.     

Nanotribological study of PECVD DLC and reactively sputtered Ti containing carbon films

Amorphous carbon film, also known as DLC film, is a promising material for tribological application. It is noted that properties relevant to tribological application change significantly depending on the method of preparation of these films. These properties are also altered by the compositions of these films. DLC films are well known for their self-lubricating properties, as well. In view of this, the objective of the present work is to compare the tribological properties of diamond like carbon (DLC) film obtained by plasma enhanced chemical vapour deposition (PECVD) with the Ti containing nanocrystalline carbon (Ti/a-C:H) film obtained by unbalanced magnetron sputter deposition (UMSD) in nN load range. Towards that purpose, DLC and Ti/a-C:H films are deposited on silicon substrate by PECVD and UMSD processes respectively. The microstructural features and the mechanical properties of these films are determined by scanning electron microscope (SEM), transmission electron microscope (TEM) and nano indenter. The surface topographies and the friction force surfaces of these films are evaluated by means of an atomic force microscope (AFM). The results show that although PECVD DLC film has higher elastic modulus and higher hardness than UMSD Ti/a-C:H film, the surface roughness and the friction coefficient of PECVD film is significantly higher than that of UMSD Ti/a-C:H film.     

The effect of annealing on mechanical and tribological properties of diamond-like carbon multilayer films

The diamond-like carbon (DLC) multilayer films have been deposited by plasma CVD deposition onSi wafer substrate. The deposited films have then been post-annealed in vacuum at 250 °C for 2 h. Changes in internal stress, hardness, critical load, friction coefficient and wear have been investigated toassess the influence of annealing on mechanical and tribological properties of DLC multilayer films. At the same time, DLC single layerfilms are also deposited and annealed in the same method for a comparison.The results show that there is 28–33% decrease in internal stress and 10–13% decrease in hardness of theDLC single layer films after the anneal treatment. However, for the DLC multilayer films, there is 41–43% decreasein internal stress and less than 2% decrease in hardness. In addition, the annealed DLC multilayer filmhas the same friction and wear properties as that un-annealed film. This result indicates that the anneal treatment isan effective method for the DLC multilayer films to reduce the internal stress and to increase the critical load.The by-effect of the annealing, decrease of hardness and wear resistance of the multilayer film, can be restrictedby the multilayer structure.     

A superhard diamond-like carbon film

A superhard hydrogen-free amorphous diamond-like carbon (DLC) film was deposited by pulsed arc discharge using a carbon source accelerator in a vacuum of 2×10⁻⁴ Pa. The growth rate was about 15 nm/min and the optimum ion-plasma energy was about 70 eV. The impact of doping elements (Cu, Zr, Ti, Al, F(Cl), N) on the characteristics of DLC films deposited on metal and silicon substrates was studied aiming at the choice of the optimum coating for low friction couples. The microhardness of thick (≥20 μm) DLC films was studied by Knoop and Vickers indentations, medium thick DLC films (1–3 μm) were investigated using a ‘Fischerscope’, and Young's module of thin films (20–70 nm) was studied by laser induced surface acoustic waves. The bonds in DLC films were investigated by electron energy loss spectroscopy (EELS), X-ray excited Auger electron spectroscopy (XAES), and X-ray photoelectron spectroscopy (XPS). The adhesion of DLC films was defined by the scratch test and Rockwell indentation. The coefficient of friction of the Patinor DLC film was measured by a rubbing cylinders test and by a pin-on-disk test in laboratory air at about 20% humidity and room temperature. The microhardness of the Patinor DLC film was up to 100 GPa and the density of the film was 3.43–3.65 g/cm³. The specific wear rate of the Patinor DLC film is comparable to that of other carbon films.     

Microstructure and adhesion characteristics of diamond-like carbon films deposited on steel substrates

For tribological applications, the low friction coefficient and high microhardness of diamond-like carbon (DLC) films give significant advantages in cutting and forming non-ferrous materials. The inherently large residual stress of DLC films, however, prevents the depositing of thicker films. This study designed and implemented a compound interface, comprising a series of metal, metal nitride, and metal carbonitride interlayers deposited in a graded structure, between the DLC (a metal-doped a-C:H) film and M2 steel substrates. The tribological performance of the interface was evaluated using a scratch tester and ball-on-disk tribometer. Meanwhile, the failure mechanism of DLC deposited on M2 steel substrates was examined using SEM/EDS and TEM microscopy. Experimental results demonstrate an improved DLC hard coating with superior adhesion strength on the steel substrates.     

The effect of nitrogen addition on field emission of diamond-like carbon films

Diamond-like carbon (DLC) films and nitrogen-doped DLC (N-DLC) films were deposited on a molybdenum-coated ceramic substrate using the pulsed laser deposition technique. The structure and surface morphology of the films were examined using X-ray diffraction, Raman spectroscopy, Auger electron spectroscopy and scanning electron microscopy. Field emission measurements were carried out, with the DLC or the N-DLC films as the cathode and ITO-coated glass as the anode. The field emission measurements indicated that the nitrogen doping could lower the turn-on field and increase the current density. It was believed that the interface at the molybdenum–N-DLC film plays an important role in improving the field emission performance of the N-DLC film.     

Stresses in diamond-like carbon films

Internal stresses have been measured in diamond-like carbon (DLC) films deposited by d.c. plasma assisted chemical vapor deposition from methane, acetylene, or cyclohexane, and in nitrogen containing DLC films deposited from acetylene, or cyclohexane and nitrogen. The total hydrogen content in the films and the fraction of bound hydrogen have been analyzed by forward recoil elastic scattering and Fourier transform infrared spectroscopy respectively. It was found that in pure DLC films the stresses increase with increasing fraction of unbound hydrogen. The highest compressive stresses were obtained in the films deposited from methane and the lowest stresses in films deposited from cyclohexane. In the nitrogen containing DLC films the stresses decrease with increasing nitrogen content in the films. Stresses as low as 0.22 GPa were obtained in the films deposited from cyclohexane and nitrogen at a ratio of 1/15 in the plasma.     

Properties of diamond-like carbon films on crystalline quartz and lithium niobate

One-micron thick DLC films are deposited on Y-X cut quartz and Y-cut lithium niobate substrates using a plasma-enhanced CVD technique. From the Raman spectra, we find that the films have a small intensity ratio of ‘D’ to ‘G’ peak, indicating a high carbon sp³/sp² ratio and high hardness characteristic. The effect of accelerating a surface acoustic wave by the DLC films has been confirmed by comparing two delayed signals from two near-by delay lines. One was coated with the DLC, while the other was kept as the free quartz or lithium niobate surfaces. It is observed that the one-micron thick DLC films are able to speed up SAW by 2.4% (at 198 MHz) for DLC/quartz and 2.5% (at 430 MHz) for DLC/lithium niobate samples, respectively.     

Tribological properties of DLC films with different hydrogen contents in water environment

Diamond-like carbon (DLC) films were deposited on silicon wafers by thermal electron excited chemical vapor deposition (CVD). To change the hydrogen content in film, we used three types of carbon source gas (C₇H₈, CH₄, and a CH₄+H₂) and two substrate bias voltages. The hydrogen content in DLC films was analyzed using elastic recoil detection analysis (ERDA). Tribological tests were conducted using a ball-on-plate reciprocating friction tester. The friction surface morphology of DLC films and mating balls was observed using optical microscopy and laser Raman spectroscopy.Hydrogen content in DLC films ranged from 25 to 45 at.%. In a water environment, the friction coefficient and specific wear rate of DLC films were 0.07 and in the range of 10⁻⁸–10⁻⁹ mm³/Nm, respectively. The friction coefficient and specific wear rate of DLC film in water were hardly affected by hydrogen content. The specific wear rate of DLC film with higher hardness was lower than that of film with low hardness. Mating ball wear was negligible and the friction surface features on the mating ball differed clearly between water and air environments, i.e., the friction surface on mating balls in water was covered with more transferred material than that in air.     

Surface acoustic waves in diamond-like carbon films on LiNbO3

Diamond-like carbon (DLC) films have been reliably deposited on YZ LiNbO_3, and surface acoustic wave (SAW) velocity change has been observed. These relatively thin films increase the SAW velocity sufficiently, and they can be used for SAW devices. The cut-off behavior was observed at approximately 538 MHz in a 2-μm-thick DLC film on the LiNbO₃ substrate.     

Effect of carbonitriding temperature process on the adhesion properties of diamond like-carbon coatings deposited by PECVD on austenitic stainless steel

The deposition of adherent coatings such as diamond-like carbon (DLC) on substrates of iron-based materials is difficult to obtain for two reasons: high residual compressive stress occurs in the inner film formation, and the mismatch of thermal expansion coefficient between steel and DLC film generates delamination effects. In order to determine the carbonitriding temperature prior to film deposition, the steel substrate and the DLC films were analyzed for their microstructure and mechanical properties of adhesion as a function of temperature. The technique used to deposit the coating was DC-pulsed plasma enhanced chemical vapor deposition. The delamination distances and the critical load of the film were obtained by scratch testing. The surface analysis by X-ray diffraction indicated the formation of nitride phases on the steel. Raman spectroscopy showed the fraction of sp³ carbon bonds in DLC films. Hardness profiling was used to verify the extent of the interface modified by carbonitriding along the cross section. For this, the steel sample with the appropriate surface modification to have high adhesion of the DLC film was used.     

Effect of nitrogen incorporation into diamond-like carbon films by ECR-CVD

Diamond-like carbon (DLC) and nitrogenated DLC (a-C:N) films were prepared on Si and glass substrates using an electron cyclotron resonance-assisted microwave plasma chemical vapour deposition (ECR-MPCVD) system with radio frequency substrate bias. The hardness and optical bandgap of the resulting films were investigated and correlated to the elemental and phase composition. The a-C:N films, deposited under conditions identical to those for the DLC films except for the introduction of a nitrogen flow, contain nitrogen which partly substitutes for hydrogen and forms carbon–nitrogen triple bonds. These bonds obstruct the formation of carbon–carbon cross-linking, resulting in softer films. These changes can be interpreted with reference to various changes of active vibronic states determined by Raman spectroscopy.     

Electrochemical behavior of the Ti–6Al–4V alloy coated with a-C:H films

In this work diamond-like carbon films were deposited on the Ti–6Al–4V alloy, which has been used in aeronautics and biomedical fields, by electrical discharges using a magnetron cathode and a 99.999% graphite target in two different atmospheres, the first one constituted by argon and hydrogen and the second one by argon and methane. Films deposited using the argon/hydrogen mixture were called a-C:H, while films deposited using the argon/methane mixture were called DLC. Raman spectroscopy was used to study the structure of the films. The Raman spectra profile of the a-C:H films is quite different from that of the DLC films. The disorder degree of the graphite crystalline phase in a-C:H films is higher than in DLC films (a-C:H films present small values for the the I_D/I_G ratio). Potentiodynamic corrosion tests in 0.5 mol l⁻¹ NaCl aqueous solution, pH 5.8, at room temperature (≈25 °C) were carried out as for the a-C:H as for the DLC coated surfaces. Comparison between the corrosion parameters of a-C:H and DLC coated surfaces under similar deposition time, showed that DLC coated surfaces present bigger corrosion potential (E_corr) and polarization resistance than those coated with a-C:H films. Electrochemical impedance spectroscopy (EIS) was also used to study the electrochemical behavior of a-C:H and DLC coated surfaces exposed to 0.5 mol l⁻¹ aqueous solution. The EIS results were simulated with equivalent electrical circuit models for porous films. The results of these simulations showed similar tendency to the one observed in the potentiodynamic corrosion tests. The DLC film resistance and the charge transfer resistance (R_ct) for the DLC coated surface/electrolyte interface were bigger than the ones determined for the a-C:H coated surfaces.     

Effect of oxygen plasma treatment on non-thrombogenicity of diamond-like carbon films

The non-thrombogenicity of oxygen-plasma-treated DLC films was investigated as surface coatings for medical devices. DLC films were deposited on polycarbonate substrates by a radio frequency plasma enhanced chemical vapor deposition method using acetylene gas. The deposited DLC films were then treated with plasma of oxygen gas at powers of 15 W, 50 W, and 200 W. Wettability was evaluated by water contact angle measurements and the changes in surface chemistry and roughness were examined by X-ray photoelectron spectroscopy and atomic force microscope analysis, respectively. Each oxygen-plasma-treated DLC film exhibited a hydrophilic nature with water contact angles of 11.1°, 17.7° and 36.8°. The non-thrombogenicity of the samples was evaluated through the incubation with platelet-rich plasma isolated from human whole blood. Non-thrombogenic properties dramatically improved for both 15 W- and 50 W-oxygen-plasma-treated DLC films. These results demonstrate that the oxygen plasma treatment at lower powers promotes the non-thrombogenicity of DLC films with highly hydrophilic surfaces.