Influence of target grit count and sintering temperature on pulsed laser deposition of SiC thin films

A pulsed laser deposition (PLD) technique for depositing SiC on Si(100) substrates using Nd³⁺:YAG laser at 355 nm is studied. The influence of substrate temperature, ambient pressure, and SiC powder grit size on both structure and morphology of SiC thin film is investigated. Further, the influence of the target preparation on the reduction of droplet formation during Nd³⁺:YAG laser-assisted pulsed laser deposition of SiC thin films is investigated. Experimental studies show that multicrystalline SiC film can be obtained with temperature ranging from 600 to 700 °C and at an ambient pressure of about 5.5 × 10^?3 Pa. Further, droplet formation on the deposited film was reduced significantly by selecting the grit count of SiC powder 500 and the pressure of 2 × 10^?2 Pa. SiC target sintered at 1,600 °C showed a reduced wear during the laser ablation. The X-ray diffraction (XRD) and the Raman spectroscopy studies on deposited films clearly show the multicrystalline (combined 3C-SiC and 4H-SiC) nature of SiC films. I-V characteristics of deposited SiC film on n-type c-Si substrate also indicated that SiC thin film possesses P-type semiconductor properties.     

Rheology of Thin Organic Films

This paper deals with the effects of contact pressure and temperature on the shear strength of thin organic films. The experimental method involves depositing the material as thin films (ca. 3 nm to 500 nm) on smooth glass surfaces. The film is sheared by sliding over it indenters of fired glass. By varying the indenter radius from 4 μm to 2.5 mm and the load from 10 mg to 20 g, the contact pressure may be varied from 10⁷ Pa (1.4 × 10³ P.s.i.) to 8 × 10⁹ Pa (12 × 10⁵ p.s.i.). The temperature dependence of the shear strength is also studied. Two types of organic materials have been investigated. These range from simple low molecular weight compounds such as stearates, to more complex high molecular weight polymers, for example P.M.M.A.

The shear strength of these films has been compared with the bulk shear properties and consideration has been given to the molecular processes occurring during shear.     

Friction of diamond-like carbon films in different atmospheres

Diamond-like carbon (DLC) films constitute a class of new materials with a wide range of compositions, properties, and performance. In particular, the tribological properties of these films are rather intriguing and can be strongly influenced by the test conditions and environment. In this paper, a series of model experiments are performed in high vacuum and with various added gases to elucidate the influence of different test environments on the tribological behavior of three DLC films. Specifically, the behavior of a hydrogen-free film produced by a cathodic arc process and two highly hydrogenated films produced by plasma-enhanced chemical-vapor deposition were studied. Flats and balls used in these experiments were coated with DLC and tested in a pin-on-disc machine under a load of 1 N and at constant rotational frequency. With a low background pressure, in the 10⁻⁶ Pa range, the highly hydrogenated films exhibited a friction coefficient of less than 0.01, whereas the hydrogen-free film gave a friction coefficient of approximately 0.6. Adding oxygen or hydrogen to the experimental environment changed the friction to some extent. However, admission of water vapor into the test chamber caused large changes: the friction coefficient decreased drastically for the hydrogen-free DLC film, whereas it increased slightly for one of the highly hydrogenated films. These results indicate that water molecules play a prominent role in the frictional behavior of DLC films—most notably for hydrogen-free films but also for highly hydrogenated films.     

Effect of atmospheric pressure on friction and wear of 0.45% C steel in fretting

Oxidative wear is significant in fretting wear when sufficient oxygen is supplied. In vacuum, however, oxide does not form readily. In this paper friction and wear behaviours were studied at various atmospheric pressures in order to clarify the effect of ambient pressure on them.Experiments were conducted with 0.45% C steel at ambient pressures from 1.0 × 10⁵ to 1.3 × 10^?3 Pa. The load was 14 N, the peak-to-peak slip amplitudes were 35 and 110 μm and the frequency was usually 8.3 Hz.Friction behaviours are characterized into three types according to the ambient pressure: 1.0 × 10⁵ ? 10 Pa, 10 ? 10^?1 Pa and below 10^?1 Pa. The coefficient of friction increases with a decrease in ambient pressure below 1 Pa. The critical pressure in fretting is found to be 10 Pa, above which the oxidation rate is independent of the ambient pressure and α-Fe₂O₃ is formed. Wear decreases with ambient pressure below the critical pressure where Fe₃O₄ is formed. Adhesive transfer of metallic debris occurs below 10^?1 Pa.The relationship between the coefficient of friction and oxide thickness is obtained analytically, and the effect of frequency on the oxidation rate is considered.     

Extremely low coefficient of friction of diamond sliding against Ag thin films on Si(1 1 1) surface under ultrahigh vacuum condition

The tribological properties of a diamond (1 1 1) pin slid on subnanometer thick Ag films, which were deposited on a cleaned Si(1 1 1) substrate, were studied using a pin-on-plate tribometer. The preparation of Ag ultrathin films and frictional experiments were performed in an ultrahigh vacuum (UHV) chamber at a pressure of 10⁻⁸ Pa. The frictional experiments were carried out at a sliding speed of 0.1 mm/s and at a normal load of 250 mN. An extremely low coefficient of friction, less than 0.01, was obtained when the pin was slid on Ag films, whose thicknesses were 1 and 2.6 monolayer (ML) under reciprocal motion. The minimum coefficient of friction was less than 0.004 for Ag 1 ML film. After the extremely low coefficient of friction was obtained, Ag remained on the worn track without any transfer to the diamond pin, as confirmed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).The mechanisms of extremely low coefficients of friction are discussed in terms of the chemical bonding force between atoms of the topmost layers, and Ag coverage on the Si surface.     

Observation of very thin gold island films vacuum-deposited onto MoS2 surface by STM

A gold film of about half a monolayer in thickness was vacuum-deposited onto air-cleaved MoS₂ surface at room temperature at a pressure of 10^?5 Pa. Quasi-two-dimensionally grown gold islands made of several atomic layers were observed by scanning an area of 40×30 nm². The shape of them was oblate and about 20 nm in diameter. Atomic corrugations which reflect the Au(111) surface were observed. The islands were found to move and changed their shape during the microscopy.     

Film Formation by Colloidal Overbased Detergents in Lubricated Contacts

It has been reported in the literature that overbased detergents can possess good antifriction and antiwear properties although the origins of these properties are not fully clear. In practice, over-based detergents are colloidal dispersions and this may be important in determining their properties and mechanism of action.

In the current study, the lubricating properties of commercial, overbased magnesium and calcium sulfonates were measured in thin film, lubricated conditions and compared to a neutral sulfonate additive. A range of techniques was employed to evaluate the tribological performance of solutions of these additives. Film thickness measurements were carried out using optical interferometry and in-contact visualization, while friction and wear measurements complemented the study.

It has been found that, when operating in thin film conditions, overbased detergents deposit solid-like boundary films on the rubbing surfaces. These films form in both rolling and mixed rolling/sliding conditions and, unlike many other colloidally-formed boundary films, are able to survive in high speed, thick film conditions. During formation, the film rapidly reaches a thickness corresponding to one colloid particle diameter, between 10 and 20 nm. After prolonged rubbing, however, the film thickness reaches the equivalent of three particle diameters. No such thick boundary films are observed with the neutral sulfonate.

The boundary films formed by overbased detergents produce a significant reduction in wear. However, for the very smooth surfaces used in this study, they also result in an effective roughening of the very smooth surfaces studied. This leads to an increase in friction in the intermediate speed region by promoting solid-solid contact in thin fluid film conditions.     

Residual gas analysis in a SEM

It is shown that a clean (hydrocarbon partial pressure 0·1 times 10^?6 Pa) high vacuum (total pressure 5 times 10^?5 Pa) is obtainable in the specimen chamber of a scanning electron microscope by relatively inexpensive means.     

Tribological behavior and tribochemical reactions of alumina in HFC-134a environment

The tribological behavior of alumina (Al₂O₃) in CF₃CH₂F (HFC-134a) gas at pressures between 170 Pa and 10⁵ Pa were investigated using a ball-on-disk type tribometer. For comparison, the friction test was also carried out in a vacuum (10⁻⁵ Pa) under the same experimental conditions. X-ray Photoelectron Spectroscopy (XPS) and Time of Flight Secondary Ions Mass Spectrometry (TOF-SIMS) were used to identify the formation of tribochemical products.It was found that the friction and wear properties of Al₂O₃ were strongly dependent on the pressure of HFC-134a gas. A higher pressure correlated to a lower friction coefficient. When the pressure exceeded 10³ Pa, the wear strikingly decreased. The results of XPS and TOF-SIMS analyses identified that tribochemical films, mainly composed of fluorine-containing organic compounds and Al-oxyfluorides, were produced on the frictional surfaces. In addition, it was found that the amount of the fluorides correlated well to the friction and wear properties, that is, the more the fluorides were, the lower were the friction and wear. The results of research indicate that HFC-134a gas has a good lubricating effect for Al₂O₃ ceramic, which is attributed to the formation of the tribofilms at the frictional interface.     

Effect of deposition pressure on microstructure and tribological behavior of MoS<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>/MoS<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>-Mo nanoscale multi-layer films

MoS _x /MoS _x -Mo multi-layer films consisted of several bilayers and a surface layer on steel substrate were deposited by d.c. magnetron sputtering at different deposition pressures. Each bilayer contained a MoS _x layer with 80 nm in thickness and a MoS _x -Mo composite layer with 20 nm in thickness. With the increase of deposition pressure, the perpendicular orientation of the basal plane prevailed while the parallel orientation decreased. The tribological properties of the multi-layer films were investigated by using a ball-on-disk tribometer both in vacuum and in humid air. The multi-layer film deposited at 0.24 Pa had a compact, consistent layered structure with high intensity of (002) plane and low S content compared to the others deposited at 0.32 and 0.40 Pa, and showed the lowest friction coefficient and wear rate in humid air.     

Equipment for deposition of thin metallic films bombarded by fast argon atoms

Deposition of thin metallic films on dielectric substrates using a source of metal atom flow combined with a flow fast argon atoms has been investigated and the investigation results are presented. The fast atoms are produced due to charge-exchange collisions in a vacuum chamber of argon ions, which are accelerated by potential difference between the hollow-cathode glow-discharge plasma and an emissive grid and enter the chamber through the grid. The metal atoms produced due to ion sputtering of a metallic foil placed on the inner surface of the hollow cathode enter the chamber through the same grid. Substrate pretreatment and pulse-periodic bombardment of the growing film by ～1-keV argon atoms both ensure adhesion of copper to glass up to 2 × 10⁷ Pa. The use of a hollow substrate holder, whose inner surface is also covered with the same foil, makes it possible to exclude losses of the depositing metal and allows recommendation of the equipment for beam-assisted deposition of precious metal films.     

An experimental study on the pumping performance of molecular drag pumps

The pumping performance of molecular drag pumps (MDP) has been investigated experimentally. The experimented MDPs are a disk-type drag pump (DTDP), helical-type drag pump (HTDP) and compound drag pump (CDP), respectively. In the case of the DTDP, spiral channels of a rotor are cut on both upper surface and lower surface of a rotating disk, and the corresponding stator is a planar disk. In the case of the HTDP, the rotor has six rectangular grooves. The CDP consists with the DTDP, at lower part, and with the HTDP, at upper part. The experiments are performed in the outlet pressure range of 0.2–533 Pa. The inlet pressure and compression ratio are measured under the various conditions of outlet pressure and throughputs, and nitrogen is used for the test gas. At the outlet pressure of 0.2 Pa, the ultimate pressure has been reached to 1.0 × 10⁻² Pa for the HTDP, 1.3 × 10⁻⁴ Pa for the DTDP, and 3.6 × 10⁻⁵ Pa for the CDP. The maximum compression ratio of the CDP is much higher than those of the DTDP or HTDP. Consequently, the ultimate pressure of the CDP is the lowest one.     

Nanosys-1000机床静压止推轴承流场分布规律及承载特性

为了提高Nanosys-1000非球面曲面光学零件超精密加工机床加工精度,研究了机床核心部件静压止推轴承内流场分布规律,进而揭示其承载特性。利用ANSYS/Fluent软件建立对称结构静压止推轴承扇形油垫的仿真模型,采用层流模式对进油压力为1.3~1.9 MPa、油膜厚度为20~36 μm的油垫流场分布规律与承载特性进行分析。研究结果表明：油垫内压力在油腔区域比较均匀,沿封油边呈线性下降;油膜承载力随油腔压力线性增长,且在同一进油压力下,油膜厚度越小,油膜承载力越大,进油压力为1.5 MPa时,油膜厚度从36 μm减小到20 μm,油腔压力从3.05×10⁵ Pa增加到8.02×10⁵ Pa,油膜承载力相应地从880 N增加到2 109 N;同一负载即油膜承载力下,进油压力越高,油膜厚度越大,油膜承载力为1 320 N时,进油压力从1.3 MPa增加到1.9 MPa,油膜厚度从26 μm增加到30 μm;同一油膜厚度下,进油压力越高,润滑油流量越大,油膜厚度为28 μm时,进油压力从1.3 MPa增加到1.9 MPa,润滑油流量从0.179 L/min增加到0.231 L/min。相关研究结果在研制的Nanosys-1000非球面曲面超精密加工机床静压止推轴承上得到了验证。     

Field emission techniques for studying surface reactions: applying them to NO-H2 interaction with Pd tips

The adsorption of NO and its reaction with H₂ over Pd tips were investigated by means of field ion microscopy (FIM) and pulsed field desorption mass spectrometry (PFDMS) in the 10⁻³ Pa pressure range and at sample temperatures between 400 and 600 K. By varying the H₂ partial pressure while keeping the other control parameters constant, the NO+H₂ reaction over Pd crystallites is shown to exhibit a strong hysteresis effect. The hysteresis region narrows with increase in temperature and the H₂ pressures delimiting this hysteresis decrease as well. Abrupt transformations of the micrographs are observed by FIM from bright to dark patterns and vice versa. These transformations define the hysteresis region. The collected data allow establishing a novel kinetic phase diagram of the NO+H₂/Pd system within the range of temperatures and pressures indicated. The observed features are correlated with a local chemical analysis by means of field pulses. NO⁺ seems to be the dominating imaging species under all conditions. At high relative H₂ pressures (the “hydrogen-side”), H atoms seem to diffuse subsurface. This process is blocked at lower H₂ pressure (the “NO-side”) due to NO_ad and O_ad accumulation on the surface. Probe-hole measurements with field pulses indicate that the Pd surface undergoes oxidation as revealed by the occurrence of PdO₂⁺ species in the mass spectra.     

Low Friction Carbide-Derived Carbon Coating on SiC in Vacuum Achieved by Microstructure Formulation and Solid–Liquid Lubrication

Carbide-derived carbon (CDC) coatings with dimple (CDC@GSiC coating) and loosely dispersive particles structures (CDC@RBSiC coating) were prepared on two kinds of SiC substrates by using chlorination at 1,000 °C in a 5 vol.% Cl₂–Ar gas. Microstructural effect makes the two CDC coatings exhibit different frictional behavior in ambient pressure and in vacuum. For the CDC@RBSiC coating, the friction coefficient was from 0.08 to 0.12 at ambient pressure and is sensitive to evacuation from ambient pressure to 10³ Pa while it was as high as 0.42 up to a pressure of 10^?4 Pa. Progressive evacuation does not vary the friction coefficient of the CDC@GSiC coating up to 10^?3 Pa. The wear of the CDC@GSiC coating was low with a maximum depth of 8 μm and much lower than that of the CDC@RBSiC coating (70 μm). The dimples on the surface and pores in the CDC@GSiC coating are reservoirs for ion liquid (IL), and the IL impregnated CDC@GSiC coating shows very low friction and wear at ambient pressure and in vacuum.     

Thin multilayer aluminum structures for superconducting devices

Various aluminum-based thin-film structures were manufactured and investigated at temperatures of 50 mK–3 K. Multilayer films of Al and Si, Al and Cr, and Al in the presence of oxygen were deposited by the thermal evaporation technique. As the thickness of pure-Al films decreases from 20 to 3 nm, the temperature of the superconducting transition increases from 1.30 to 2.45 K. An increase in the oxygen pressure to 5 × 10⁻⁶ mbar during deposition of Al films results in an increase in the critical temperature to 2.4 K. The presence of a chromium sublayer with a thickness of <0.5 nm may lead to complete suppression of superconductivity, whereas a thicker layer, 1–4 nm, deposited at a higher temperature with preliminary sputtering reduces the critical current of Al/Cr two-layer films to a lower degree. An atomic-force microscope was used to study the surface morphology and granularity and the roughness of manufactured film structures. The smallest linear roughness having a size of 0.29 nm for a 3-nm-thick film shows the advantage of using thinner films for creating a homogeneous tunneling barrier.     

溅射气压和衬底温度对Si1-xGex薄膜结构和光吸收性能的影响

采用射频磁控溅射法沉积了Si1-xGex薄膜,研究了溅射气压、衬底温度对薄膜结构、厚度、表面形貌、表面成分及光吸收性能的影响。结果表明:薄膜均为微晶结构且相组成不随溅射气压和衬底温度的改变而改变;随着溅射气压升高,薄膜结晶性能降低,升高衬底温度使其结晶性能提高;随气压或温度的升高,薄膜厚度均先增大后减小,在1.0Pa或400℃达到最大值;随温度的升高,薄膜表面团簇现象消失并变得平整致密,气压为8.0Pa时,表面有孔洞和沟道;随气压升高,薄膜中锗含量降低,光吸收强度减小,光学带隙增大;衬底温度的变化对光学带隙影响不大。     

Tribological Performance of Diamond and Diamondlike Carbon Films at Elevated Temperatures

In this study, the authors investigated the tribological performance of diamond and diamondlike carbon (DLC) films as a function of temperature. Both films were deposited on silicon carbide (SiC) by microwave plasma chemical vapor deposition and ion-beam deposition processes. Tribological tests were performed on a reciprocating wear machine in open air (20 to 30% relative humidity) and under a 10 N load using SiC pins. For the test conditions explored, the steady-state friction coefficients of test pairs without a diamond or DLC film were 0.7 to 0.9 and the average wear rates of pins were 10^?5 to 10^?7 mm³/N·m, depending on ambient temperature. DLC films reduced the steady-slate friction coefficients of the test pairs by factors of three to five and the wear rates of pins by two to three orders of magnitude. Low friction coefficients were also obtained with the diamond films, but wear rates of the counterface pins were high due to the very abrasive nature of these films. The wear of SiC disks coated with either diamond or DLC films was virtually unmeasurable while the wear of uncoated disks was substantial. Test results showed that the DLC films could afford low friction up to about 300° C. At higher temperatures, the DLC films graphitized and were removed from the surface. The diamond films could withstand much higher tempera-lures, but their tribological behavior degraded. Raman spectroscopy and scanning electron microscopy were used to elucidate the friction and wear mechanisms of both films at high temperatures.     

Nucleation and formation of oxide film with the magnetic field on dry sliding contact of ferromagnetic steel

The nucleation and formation of oxide film in unidirectional dry sliding contact has been studied in a vacuum chamber with and without the application of a magnetic field in the intention of identifying the role of magnetic intensity on the oxidation wear. The wear tests of the steel AISI 1045/steel AISI 1045 couple are investigated on a pin‐disc configuration under three various gas environments: in ambient air, under oxygen at 10⁵ Pa and in vacuum at 5.10⁻⁵ Pa. The formation of oxide layer strongly depends on oxygen partial pressure and magnetic field intensity. These took the form of protective raised ‘islands’ of compacted debris which is developed gradually but rapidly increased as the oxygen partial pressure is increased and which could persist for extended periods during subsequent evacuation. Evidence from various experimental techniques indicates that the compacted debris is a mixture of iron oxides in the form of oxide‐covered particles, although the depth of oxide film has not yet been fully elucidated. Copyright © 2010 John Wiley & Sons, Ltd.     

Microstructure, Morphology and Properties of Titanium Containing Graphite-Like Carbon Films Deposited by Unbalanced Magnetron Sputtering

A series of graphite-like carbon films with a titanium concentration of about 3.0 at.% were successfully deposited on silicon wafer substrates using an unbalanced magnetron sputtering system with different bias voltages. The microstructure, surface morphology, and properties of the titanium-containing graphite-like carbon films were subsequently studied using different characterization techniques. The results show that the resulting titanium-containing graphite-like carbon films are completely dominated by sp² sites and that these films have moderate hardness, low internal stress, and superior tribological properties with low friction and a high load-bearing capacity. The hardness (H), elastic modulus (E), H/E, H ³/E ², and internal stress of the titanium-containing graphite-like carbon films initially increase with increasing bias voltage, only to be followed by a decrease with further increases in the bias voltage. Tribologically, the studied carbon film shows a slight increase in friction with increasing bias voltage, while the wear rate initially decreases, followed by an obvious increase. The tribological properties of the studied titanium-containing graphite-like carbon films are greatly improved under the liquid paraffin-lubricated condition, achieving extremely low friction (~0.045) and wear (~10^?9 mm³/Nm). The effect of bias voltage on the microstructure and properties of the titanium-containing graphite-like carbon films is discussed in detail.