Thin films of diamond-like carbon(DLC) have been deposited using a magnetron plasma-enhanced chemical vapor deposition(PECVD) method with an rf(13.56 MHz) plasma of $C_{3}H_{8}$. From the Langmuir probe I-V characteristics, it can be observed that increasing the magnetic field yields an increase of the temperature($T_e$) and density($N_e$) of electron. At a magnetic field of 82 Gauss, the estimated values of $T_e$ and $N_e$ are approximately $1.5\;{\times}\;10^5$ K(13.5 eV) and $1.3\;{\times}\;10^{11}\;cm^{-3}$, respectively. Such a highly dense plasma can be attributed to the enhanced ionization caused by the cyclotron motion of electrons in the presence of a magnetic field. On the other hand, the negative dc self-bias voltage($-V_{sb}$) decreases with an increasing magnetic field, which is irrespective of gas pressure in the range of $1{\sim}7$ mTorr. This result is well explained by a theoretical model considering the variation of $T_e$. Deposition rates of DLC films increases with a magnetic field. This may be due to the increased mean free path of electrons in the magnetron plasma. Structures of DLC films are examined by using various techniques such as FTIR and Raman spectroscopy. Most of hydrocarbon bonds in DLC films prepared consist of $sp^3$ tetrahedral bonds. Increasing the rf power leads to an enhancement of cross-linking of carbon atoms in DLC films. At approximately 140 W, the maximum film density obtained is about 2.4 $g/cm^3$.
The silicon-containing Diamond-like Carbon (Si-DLC) film as an low friction coefficient coating has especially treated a different silicon content by plasma-enhanced chemical vapor deposition (PECVD) process at $500^{\circ}C$ on nitrided-STD 11 mold steel with (TMS) gas flow rate. The effects of variable silicon content on the Si-DLC films were tested with relative humidity of 5, 30 and 85% using a ball-on-disk tribometer. The wear-tested and original surface of Si-DLC films were analysed for an understanding of physical and chemical characterization, including a changing structure, via Raman spectra and nano hardness test. The results of Raman spectra have inferred a changing intra-structure from dangling bonds. And high silicon containing DLC films have shown increasing carbon peak ratio ($I_D/I_G$) values and G-peak values. In particular, the tribological tested surface of Si-DLC was shown the increasing hardness value in proportional to TMS gas flow rate. Therefore, at same time, the structure of the Si-DLC film was changed to a different intra-structure and increased hardness film with mechanical shear force and chemical reaction.
In this study, the electrical conductivity, transmittance and gas barrier properties of diamond-like carbon (DLC) thin films were studied. DLC is an insulator, and has transmittance and oxygen gas barrier properties varying depending on the thickness of the thin film. Recently, many researchers have been trying to apply DLC properties to specific industrial conditions. The DLC thin films were deposited by PECVD (Plasma Enhanced Chemical Vapor Deposition) process. The doping gas was used for the DLC film to have electrical conductivity, and the optimum conditions of transmittance and gas barrier properties were established by adjusting the gas ratio and DLC thickness. In order to improve the electrical conductivity of the DLC thin film, $N_2$ doping gas was used for $CH_4$ or $C_2H_2$ gas. Then, a heat treatment process was performed for 30 minutes in a box furnace set at $200^{\circ}C$. The lowest sheet resistance value of the DLC film was found to be $18.11k{\Omega}/cm^2$. On the other hand, the maximum transmittance of the DLC film deposited on the PET substrate was 98.8%, and the minimum oxygen transmission rate (OTR) of the DLC film of $C_2H_2$ gas was 0.83.
Amorphous carbon (a-C) has excellent wear resistance and, therefore is used as a coating to protect numerous mechanical components to prolong their lifetimes. Among the a-C coatings, diamond-like carbon (DLC) and DLC-containing silicon (Si-DLC) receive extensive attention owing to their enhanced wear resistance and low frictional characteristics. In this study, the friction and wear characteristics of DLC and Si-DLC coatings are analyzed. For comparative analysis, DLC-coated and Si-DLC-coated vanes are utilized with the counterpart of a roller for the friction tests. Since the lubricated mechanical components are generally vulnerable to wear when a lubricant film does not form properly, friction tests are conducted under boundary lubrication conditions to promote wear. A cylinder-on-cylinder type tribometer is used to perform the friction tests with various normal load conditions. After the friction test, a 3D laser confocal microscope is used for quantifying the wear volume to calculate the wear rate of each specimen. Consequently, the DLC-coated specimen shows a lower coefficient of friction (COF) and wear rate than the specimen without the coating, while the Si-DLC coating shows a higher COF than the bare specimen. The results of this study are expected to contribute to improving the efficiency and reliability of compressors.
Lee, Woo Young;Ryu, Ho Jun;Jang, Young Jun;Kim, Gi Taek;Deng, Xingrui;Umehara, Noritsugu;Kim, Jong Kuk
한국진공학회:학술대회논문집
/
한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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pp.144.2-144.2
/
2016
Diamond-like carbon (DLC) coatings have been widely applied to the mechanical components, cutting tools due to properties of high hardness and wear resistance. Among them, hydrogenated amorphous carbon (a-C:H) coatings are well-known for their low friction properties, stable production of thin and thick film, they were reported to be easily worn away under high temperature. Non-hydrogenated tetrahedral amorphous carbon (ta-C) is an ideal for industrial applicability due to good thermal stability from high $sp^3$-bonding fraction ranging from 70 to 80 %. However, the large compressive stress of ta-C coating limits to apply thick ta-C coating. In this study, the thick ta-C coating was deposited onto Inconel alloy disk by the FCVA technique. The thickness of the ta-C coating was about $3.5{\mu}m$. The tribological behaviors of ta-C coated disks sliding against $Si_3N_4$ balls were examined under elevated temperature divided into 23, 100, 200 and $300^{\circ}C$. The range of temperature was setting up until peel off observed. The experimental results showed that the friction coefficient was decreased from 0.14 to 0.05 with increasing temperature up to $200^{\circ}C$. At $300^{\circ}C$, the friction coefficient was dramatically increased over 5,000 cycles and then delaminated. These phenomenon was summarized two kinds of reasons: (1) Thermal degradation and (2) graphitization of ta-C coating. At first, the reason of thermal degradation was demonstrated by wear rate calculation. The wear rate of ta-C coatings showed an increasing trend with elevated temperature. For investigation of relationship between hardness and graphitization, thick ta-C coatings(2, 3 and $5{\mu}m$) were additionally deposited. As the thickness of ta-C coating was increased, hardness decreased from 58 to 49 GPa, which means that graphitization was accelerated. Therefore, now we are trying to increase $sp^3$ fraction of ta-C coating and control the coating parameters for thermal stability of thick ta-C at high temperatures.
Atomic force microscopy/friction force microscopy (AFM/FFM) techniques are increasingly used for tribological studies of engineering surfaces at scales, ranging from atomic and molecular to microscales. These techniques have been used to study surface roughness, adhesion, friction, scratching/wear, indentation, detection of material transfer, and boundary lubrication and for nanofabrication/nanomachining purposes. Micro/nanotribological studies of single-crystal silicon, natural diamond, magnetic media (magnetic tapes and disks) and magnetic heads have been conducted. Commonly measured roughness parameters are found to be scale dependent, requiring the need of scale-independent fractal parameters to characterize surface roughness. Measurements of atomic-scale friction of a freshly-cleaved highly-oriented pyrolytic graphite exhibited the same periodicity as that of corresponding topography. However, the peaks in friction and those in corresponding topography were displaced relative to each other. Variations in atomic-scale friction and the observed displacement has been explained by the variations in interatomic forces in the normal and lateral directions. Local variation in microscale friction is found to correspond to the local slope suggesting that a ratchet mechanism is responsible for this variation. Directionality in the friction is observed on both micro- and macro scales which results from the surface preparation and anisotropy in surface roughness. Microscale friction is generally found to be smaller than the macrofriction as there is less ploughing contribution in microscale measurements. Microscale friction is load dependent and friction values increase with an increase in the normal load approaching to the macrofriction at contact stresses higher than the hardness of the softer material. Wear rate for single-crystal silicon is approximately constant for various loads and test durations. However, for magnetic disks with a multilayered thin-film structure, the wear of the diamond like carbon overcoat is catastrophic. Breakdown of thin films can be detected with AFM. Evolution of the wear has also been studied using AFM. Wear is found to be initiated at nono scratches. AFM has been modified to obtain load-displacement curves and for nanoindentation hardness measurements with depth of indentation as low as 1 mm. Scratching and indentation on nanoscales are the powerful ways to screen for adhesion and resistance to deformation of ultrathin fdms. Detection of material transfer on a nanoscale is possible with AFM. Boundary lubrication studies and measurement of lubricant-film thichness with a lateral resolution on a nanoscale have been conducted using AFM. Self-assembled monolyers and chemically-bonded lubricant films with a mobile fraction are superior in wear resistance. Finally, AFM has also shown to be useful for nanofabrication/nanomachining. Friction and wear on micro-and nanoscales have been found to be generally smaller compared to that at macroscales. Therefore, micro/nanotribological studies may help def'me the regimes for ultra-low friction and near zero wear.
Nano/micro friction with the contact area was studied on Si-wafer (100) and diamond-like carbon (DLC) film. Borosilicate balls of radii $0.32{\mu}m,\;0.5{\mu}m,\;1.25{\mu}m\;and\;2.5{\mu}m$ mounted on the top of AFM tip (NPS) were used for nano-scale contact and Soda Lime glass balls of radii 0.25mm, 0.5mm, 1mm were used for micro-scale contact. At nano-scale, the friction between ball and surface was measured with the applied normal load using an atomic force microscope (AFM), and at micro scale it was measured using ball-on flat type micro-tribotester. All the experiments were conducted at controlled conditions of temperature $(24\pm1^{\circ}C)$ and humidity $(45\pm5\%)$. Friction was measured as a function of applied normal load in the range of 0-160nN at nano scale and in the range of $1000{\mu}N,\; 1500{\mu}N,\;3000{\mu}N\;and\;4800{\mu}N$ at micro scale. Results showed that the friction at nano scale increased with the applied normal load and ball size for both kinds of samples. Similar behavior of friction with the applied normal load and ball size was observed for Si-wafer at micro scale. However, for DLC friction decreased with the ball size. This difference of in behavior of friction in DLC nano- and microscale was attribute to the difference in the operating mechanisms. The evidence of the operating mechanisms at micro-scale were observed using scanning electron microscope (SEM). At micro-scale, solid-solid adhesion was dominant in Silicon-wafer, while plowing in DLC. Contrary to the nano scale that shows almost a wear-less situation, wear was prominent at micro-scale. At nano- and micro-scale, effect of contact area on the friction was discussed with the different applied normal load and ball size.
Surface engineering plays a significant role in fabricating highly functionalized materials applicable to industrial and biomedical fields. Surface wrinkles and folds formed by ion beam or plasma treatment are buckling-induced patterns and controlled formation of those patterns has recently gained considerable attention as a way of creating well-defined surface topographies for a wide range of applications. Surface wrinkles and folds can be observed when a stiff thin layer attached to a compliant substrate undergoes compression and plasma treatment is one of the techniques that can form stiff thin layers on compliant polymeric substrates, such as poly (dimethylsiloxane) (PDMS). Here, we report two effective methods using plasma modification techniques for controlling the formation of surface wrinkles and folds on flat or patterned PDMS substrates. First, we show a method of creating wrinkled diamond-like carbon (DLC) film on grooved PDMS substrates. Grooved PDMS substrates fabricated by a molding method using a grooved master prepared by photolithography and a dry etching process were treated with argon plasma and subsequently coated with DLC film, which resulted in the formation of wrinkled DLC film aligning perpendicular to the steps of the pre-patterned ridges. The wavelength and the amplitude of the wrinkled DLC film exhibited variation in the submicron- to micron-scale range according to the duration of argon plasma pre-treatment. Second, we present a method for controlled formation of folds on flat PDMS substrates treated with oxygen plasma under large compressive strains. Flat PDMS substrates were strained uniaxially and then treated with oxygen plasma, resulting in the formation of surface wrinkles at smaller strain levels, which evolved into surface folds at larger strain levels. Our results demonstrate that we can control the formation and evolution of surface folds simply by controlling the pre-strain applied to the substrates and/or the duration of oxygen plasma treatment.
The liquid-phase sintering method was used to prepare a glass lens forming core composed of SiC-$Al_2O_3-Y_2O_3$. Spark plasma sintering was used to obtain dense sintered bodies. The sintering characteristics of different SiC sources and compositions of additives were studied. Results revealed that, owing to its initial larger surface area, $\alpha$-SiC offers sinterability that is superior to that of $\beta$-SiC. A maximum density of $3.32\;g/cm^3$ (theoretical density [TD] of 99.7%) was obtained in $\alpha$-SiC-10 wt% ($6Al_2O_3-4Y_2O_3$) sintered at $1850^{\circ}C$ without high-energy ball milling. The maximum hardness and compression stress of the sintered body reached 2870 Hv and 1110 MPa, respectively. The optimum ultra-precision machining parameters were a grinding speed of 1243 m/min, work spindle rotation rate of 100 rpm, feed rate of 0.5 mm/min, and depth of cut of $0.2\;{\mu}m$. The surface roughnesses of the thus prepared final products were Ra = 4.3 nm and Rt = 55.3 nm for the aspheric lens forming core and Ra = 4.4 nm and Rt = 41.9 for the spherical lens forming core. These values were found to be sufficiently low, and the cores showed good compatibility between SiC and the diamond-like carbon (DLC) coating material. Thus, these glass lens forming cores have great potential for application in the lens industry.
In order to characterize the adhesive properties and failure mechanisms of diamond-like carbon (DLC) films of two different thicknesses (130 nm and $1.2{\mu}m$), deposited by plasma-enhanced chemical vapor deposition on a Si substrate, scratch testing with a micro-indenter ($12.5{\mu}m$ tip radius) was performed under a linearly increasing load. These scratch tests were conducted under the same test conditions for both films. The critical load of each film was estimated from the scratch test results, based on a sharp increase in the coefficient of friction and a clear distinction of failure modes. The critical load was the basis for evaluating the adhesion strength of the films, and the $1.2{\mu}m-thick$ DLC film had superior adhesion strength. For better understanding of the failure modes, the following analyses were conducted: friction behavior and scratch tracks analysis using scanning electron microscopy, energy-dispersive spectroscopy, and 3-D profilometry. The scratch test results showed that failure modes were related to the thickness of the films. The 130 nm-thick DLC film underwent cohesive failure modes (cracks and chipping) before reaching to a gross failure stage. On the other hand, the thicker DLC film ($1.2{\mu}m-thick$) did not exhibit micro cracks before a sudden gross failure of the film together with the evidence of cracking and chipping of the Si substrate.
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