Effects of proton and electron irradiation on the structural and tribological properties of MoS2/polyimide

To study the structural and tribological properties of MoS₂/polyimide (MoS₂/PI) composite under the irradiation environment of proton and electron, the MoS₂/PI composites were investigated in a ground-based simulation facility, in which the energy of proton and electron was 25 keV and the flux was 2.5 × 10¹⁴ cm⁻² s⁻¹. The experimental results revealed that the simplex and combined irradiation of proton and electron induced bond break and cross-link, proton irradiation can break the PI bond easier than electron irradiation and then formed the graphite-like structure at surface area of the samples. Irradiation decreased the friction coefficient and wear rate remarkably of the composites comparing with the pristine one. The wear rate increased with the increasing of the proton and combined radiation time, and decreased with the electron radiation conditions.     

Tribological properties of the Ti-Al-N thin films with different components fabricated by double-targeted co-sputtering

Ti-Al-N films with different chemical compositions were deposited on stainless steel by changing the relative substrate position to targets using double-targeted reactive magnetron sputtering technique in the same process. The tribological behavior of the Ti-Al-N films was investigated in the temperature ranging from room temperature to elevated temperature in air without any lubricant on UMT-3 multifunctional friction and wear tribometer. The structure of the as-deposited films and the worn surface after tribometer testing were identified using XRD, EDS and SEM. It was found that the chemical composition of the as-deposited films altered with substrate position from Ti_0.82Al_0.18N to Ti_0.12Al_0.88N. XRD results revealed that the sputtered films before heat treatment were amorphous, but different phases such as TiN, AlN and TiAlN were formed after heat treatment of 700 °C × 1 h. Friction and wear tests indicated the films with x = 0.57, 0.65 exhibited the best tribological performance during the Ti_1−xAl_xN films system because of its hard phase and the formation of transfer films.     

Fabrication and tribological properties of super-hydrophobic surfaces based on porous silicon

In the present work, super-hydrophobic surfaces based on porous silicon (PS) were constructed by the self-assembled molecular films and their tribological properties were investigated. A simple chemical etching approach was developed to fabricate PS with the certain rough microstructure surface, which can be observed by the environmental scanning electron microscopy (ESEM). The hydrocarbon and fluorocarbon alkylsilane molecular films were self-assembled on PS, which was confirmed by the X-ray photoelectron spectroscopy (XPS) measurement. In contrast to PS, the alkylsilane molecular films modified PS (mPS) were super-hydrophobic since the apparent water contact angle (CA) exceeded 160°. The tribological properties of PS and the mPS were investigated by a ball-on-disk tribometer during the processes of different sliding velocities and normal loads. The experimental results showed that the alkylsilane molecular films could decrease the friction coefficient. Due to the difference of chain structure and functional groups, the fluorinated alkylsilane films are better candidates for improving the hydrophobicity and lubricating characteristics of PS comparing to the non-fluorinated ones. The carbon chain length of alkylsilane molecules self-assembling on the Si or PS substrates could have little effects on the hydrophobic properties and the tribology performances.     

The properties of copper films deposited on polyimide by nitrogen and oxygen plasma pre-treatment

Extensive studies on the relationship between a copper thin film and its polyimide substrate show that the adhesion strength is very weak. In this work, we show how to reduce Cu film resistivity and improve the adhesion strength between Cu and polyimide. After nitrogen and oxygen plasma treatment, polyimide substrates can substantially improve the resistivity and adhesion strength deposited Cu. It is found that the lowest resistivity is 4.22 μΩ cm and the maximum adhesion strength is 72.23 MPa for a polymide substrate treated in oxygen plasma for 5 min.     

分层蒸镀制备聚酰亚胺自支撑膜及其特性研究

 采用分层蒸镀法,在玻璃基片上依次蒸镀二氨基二苯醚（ODA）和均苯四甲酸二酐（PMDA）两种单体,然后在空气环境中对样品进行不同温度和时间的热亚胺化处理,使二者在交界面上反应生成聚酰亚胺。经加热150 ℃ 1 h然后经350 ℃ 2 h处理的样品,在脱膜后能制备出直径1.8 cm,厚度为100 nm的聚酰亚胺自支撑薄膜。用FTIR测量了自支撑薄膜的红外光谱,特征吸收峰的分析表明薄膜已基本上完全亚胺化。用原子力显微镜分析了浮法玻璃衬底上聚酰亚胺薄膜的表面形貌,结果表明以ODA作为内层制备的膜层表面更光滑平整。     

Influences of ultraviolet irradiation on structure and tribological properties of diamond-like carbon films

Two types of diamond-like carbon (DLC) films with different bonding configurations were produced by pulse-assisted and DC-assisted plasma chemical vapor deposition. The chemical composition, surface morphology, microstructure, internal stress and tribological properties of the two films before and after the ultraviolet (UV) irradiation were investigated and compared. It was found that the UV irradiation had little effects on the chemical composition and surface morphology of both the films, but greatly influenced their tribological properties in the opposite trends. This result was attributed to the different changing outcomes of the bonding configuration induced by the UV actions of primary photo-dissociation and secondary recombination, wherein the inherent bonding configuration and internal stress played important roles.     

Influence of adhesive layer properties on laser-generated ultrasonic waves in thin bonded plates

This paper studies quantitatively the generation of Lamb waves in thin bonded plates subjected to laser illumination, after considering the viscoelasticity of the adhesive layer. The displacements of such plates have been calculated in the frequency domain by using the finite element method, and the time domain response has been reconstructed by applying an inverse fast Fourier transform. Numerical results are presented showing the normal surface displacement for several configurations: a single aluminum plate, a three-layer bonded plate, and a two-layer plate. The characteristics of the laser-generated Lamb waves for each particular case have been investigated. In addition, the sensitivity of the transient responses to variations of material properties (elastic modulus, viscoelastic modulus, and thickness) of the adhesive layer has been studied in detail.     

Characteristics of ZnO-Cu-ZnO multilayer films on copper layer properties

ZnO/Cu/ZnO multilayers on glass with different copper layer thickness were prepared by simultaneous RF magnetron sputtering of ZnO and dc magnetron sputtering of Cu. Different optimization procedure were used for good transparent conductive film. Several analytical tools such as spectrophotometer, scanning electron microscope (SEM), four point probes were used to explore the causes of the changes in electrical and optical properties. The sheet resistance of the structure was severely influenced by the deposition condition of both top ZnO and intermediate Cu layer. Effect of substrate temperature and annealing treatment on ZnO and Cu layer was analyzed. A sheet resistance of 10 Ω/sq and transmittance over 85% at 580 nm wavelength was achieved and could be reproduced by controlling the preparation process parameter. The results of an optimization condition of both oxide layers and metallic Cu layers are illustrated.     

Structure and tribological properties of amorphous carbon films deposited by electrochemical method on GCr15 steel substrate

Amorphous carbon films were deposited on GCr15 steel substrates by electrolysis of methanol, dimethylsulfoxide (DMSO) and the methanol-DMSO intermixture electrolytes, respectively, under high voltage and low temperature conditions. The microstructure and wear morphology of the deposited films were analyzed using X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectrometer (EDX), respectively. The tribological properties of the films were evaluated using a ball-on-disk rotating friction tester under dry friction condition. The results show that the films deposited by electrodeposition technique on GCr15 steel substrates are amorphous carbon films. It is also found that the electrolytes have an obvious influence on the tribological properties of the deposited films with the electrodeposition method. The tribological properties of the films deposited with the intermixture electrolyte are better than those of the films deposited by other pure electrolytes. The related growth mechanism of the films in the liquid-phase electrodeposition is discussed as well in this study. Via the reaction of the CH₃ groups with each other to form carbon network and reaction of the CH₃ and SO²⁺ groups to achieve the doping of sulfur atom in the carbon network, respectively, in other words, amorphous carbon films can be obtained on GCr15 steel substrates by electrodeposition technique.     

Study on structural properties of epitaxial silicon films on annealed double layer porous silicon

In this paper, epitaxial silicon films were grown on annealed double layer porous silicon by LPCVD. The evolvement of the double layer porous silicon before and after thermal annealing was investigated by scanning electron microscope. X-ray diffraction and Raman spectroscopy were used to investigate the structural properties of the epitaxial silicon thin films grown at different temperature and different pressure. The results show that the surface of the low-porosity layer becomes smooth and there are just few silicon-bridges connecting the porous layer and the substrate wafer. The qualities of the epitaxial silicon thin films become better along with increasing deposition temperature. All of the Raman peaks of silicon films with different deposition pressure are situated at 521 cm⁻¹ under the deposition temperature of 1100 °C, and the Raman intensity of the silicon film deposited at 100 Pa is much closer to that of the monocrystalline silicon wafer. The epitaxial silicon films are all (4 0 0)-oriented and (4 0 0) peak of silicon film deposited at 100 Pa is more symmetric.     

Improving the conductivity of diamond-like carbon films with zinc doping and its material properties

Zinc doped diamond-like carbon (DLC) nanocomposite thin films are fabricated by KrF pulsed laser deposition. Carbon targets containing 3.0, 5.0 and 10.0 atomic percentages of zinc are used as the source for the laser system. Investigation of electrical properties by the four-point probe shows that doping zinc into DLC can lower the electrical sheet resistivity. Microstructural analysis by Raman spectroscopy and XPS show a lower sp³ content but a higher SiC content with an increasing amount of zinc incorporation. The increase of SiC leads to an increase in adhesion strength. Surface roughness of the films also increases while the coefficients of friction for the films do not change.     

Modification of the surface properties of polyimide films using polyhedral oligomeric silsesquioxane deposition and oxygen plasma exposure

Topographically rich surfaces were generated by spray-coating organic solutions of a polyhedral oligomeric silsesquioxane, octakis(dimethylsilyloxy)silsesquioxane (POSS), on Kapton^® HN films and exposing them to radio frequency generated oxygen plasma. Changes in both surface chemistry and topography were observed. High-resolution scanning electron microscopy indicated substantial modification of the POSS-coated polyimide surface topographies as a result of oxygen plasma exposure. Water contact angles varied from 104° for unexposed POSS-coated surfaces to ∼5° for samples exposed for 5 h. Modulation of the dispersive and polar contributions to the surface energy was determined using van Oss Good Chaudhury theory. Changes in surface energy are related to potential adhesive interactions with lunar dust simulant particles.     

Influence of sulfidation treatment on the structure and tribological properties of nitrogen-doped diamond-like carbon films

The nitrogen-doped diamond-like carbon (DLC) films were deposited on high speed steel (HSS) substrates in the direct current unbalanced magnetron sputtering system. Sulphurized layer was formed on the surface of DLC films by means of liquid sulfidation in the intermixture of urea and thiourea solution in order to improve the tribological properties of DLC films. The influence of sulfidation treatment on the structure and tribological properties of DLC films was investigated in this work. The structure and wear surface morphology of DLC films were analyzed by Raman spectroscopy, XPS and SEM, respectively. It reveals that the treated films are smooth and uniform; and sulfur atoms are bonded chemically. The treated films have broader distribution of Raman spectra in the range of 1000-1800 cm⁻¹ and higher I_D/I_G ratio than the untreated films as a result of the appearance of the crystalline graphite structure after the sulfidation treatment. It is showed that the sp² relative content increase in the treated films from the XPS measurement. The Raman results are consistent with the XPS results. The tribological properties of DLC films were investigated using a ball-on-disk rotating friction and wear tester under dry friction conditions. It is found that the sulfidation concentration plays an important part in the tribological properties of the treated DLC films. The results showed the treated films with low sulfidation concentration have a lower friction coefficient (0.1) than the treated films with high sulfidation concentration (0.26) and the untreated films (0.27) under the same friction testing conditions, which can be attributed to both the presence of sulfur-containing materials and the forming of the mechanical alloyed layer on the wear surface. Adding the dry nitrogen to the sliding surface in the testing system helps the friction coefficient of the treated films with low sulfidation concentration to decrease to 0.04 further in this work. On the basis of the experimental results, it is indicated that the liquid sulfidation technique, which is low-cost, non-polluting and convenience, would be an appropriate method for the surface treatment of DLC films.     

Epitaxial growth of cadmium telluride films on silicon with a buffer silicon carbide layer

An epitaxial 1–3-μm-thick cadmium telluride film has been grown on silicon with a buffer silicon carbide layer using the method of open thermal evaporation and condensation in vacuum for the first time. The optimum substrate temperature was 500°C at an evaporator temperature of 580°C, and the growth time was 4 s. In order to provide more qualitative growth of cadmium telluride, a high-quality ~100-nm-thick buffer silicon carbide layer was previously synthesized on the silicon surface using the method of topochemical substitution of atoms. The ellipsometric, Raman, X-ray diffraction, and electron-diffraction analyses showed a high structural perfection of the CdTe layer in the absence of a polycrystalline phase.

     

气相沉积法制备聚酰亚胺薄膜不同单体配比的表征及其性能影响

聚酰亚胺微球作为惯性约束聚变的重要候选靶丸之一,其力学性能和热学性能的提高对于实现聚变点火有重要意义.本文以均苯四甲酸二酐和二氨基二苯醚为原料,采用气相沉积法制备了不同单体配比的聚酰胺酸薄膜,研究了制备聚酰胺酸薄膜过程中不同单体蒸发温度对薄膜组成的影响,并对聚酰胺酸薄膜进行热环化处理.采用红外光谱仪分析了聚酰胺酸薄膜和聚酰亚胺薄膜的组成,结果表明:随着二酐蒸发温度的增加,聚酰胺酸薄膜中过量二酐单体的红外吸收振动特征峰(1780 cm~(-1),1850 cm~(-1)强度增加,单体配比由二胺过量到二酐二胺配比均衡再到二酐过量.热环化处理的过程中,薄膜中过量单体会再次蒸发,其红外图谱显示最终产物只有聚酰亚胺,但单体配比接近样品聚酰亚胺红外特征振动峰(1380 cm~(-1))强度更大.X射线衍射图谱显示配比接近的样品具有更高的晶化程度,说明过量单体的存在抑制了聚酰胺酸分子链的生长,造成分子量降低.采用纳米压痕仪和热重分析仪分别测量了聚酰亚胺薄膜的弹性模量和硬度以及失重曲线,结果表明分子量的降低会造成聚酰亚胺薄膜的弹性模量和硬度的降低,同时热稳定性也变差.扫描电子显微镜图像显示聚酰亚胺薄膜呈层状结构,单体配比接近的样品表面状况更好,这一点与聚酰亚胺分子的生长规律相符合.     

Physical properties of ZnSe thin films deposited on glass and silicon substrates

ZnSe thin films were deposited onto Corning glass and silicon substrates using thermal evaporation. The samples were prepared at different substrate temperatures. The thin films’ surface chemical composition was determined through Auger electron spectroscopy (AES). AES signals corresponding to Zn and Se were only detected in AES spectra. The samples’ crystallographic structure was studied through X-ray diffraction. The material crystallised in the cubic structure with preferential orientation (111). Optical properties of the ZnSe films were studied over two energy ranges via electron energy loss spectroscopy (10–90 eV) and spectral transmittance measurements (0.4–4 eV). In both cases, the spectral variation of the refractive index and the absorption coefficient were determined by fitting the experimental results with well-established theoretical models. Experimental values for the material’s gap were also found, and photoconductivity (PC) measurements were carried out. Transitions between bands, usually labelled Γ^V₈ → Γ^C₆ and Γ^V₇ → Γ^C₆, were found in the optical and PC responses. A wide spectral photoconductive response between 300 and 850 nm was found in the ZnSe/Si samples prepared at 250 °C substrate temperature.     

Structural and tribological properties of nitrogen doped amorphous carbon thin films synthesized by CFUBM sputtering method for protective coatings

Nitrogen doped amorphous carbon (a-C:N) films are a material that may successfully compete with DLC coatings, which have high hardness, high wear resistance, and a low friction coefficient. The a-C:N films were prepared on silicon substrate by a closed-field unbalanced magnetron sputtering method with a graphite target and using the Ar/N₂ mixture gases. And, we investigated the effects of various DC bias voltages from 0 to −300 V on the structural and tribological properties of the a-C:N films. This study was focused on improving physical properties of the a-C:N film by controlling process parameters like negative substrate DC bias voltage. The maximum hardness of the a-C:N film was 23 GPa, the friction coefficient was 0.08, and the critical load was 25 N on a Si wafer. Consequently, the structural and tribological properties of the a-C:N film showed a clear dependence on the energy of ions bombardment and the density of the sputtering and the reaction gases during film growth.     

Influence of silicon on the microstructure and mechanical properties of Zr-Si-N composite films

A series of Zr-Si-N composite films with different Si contents were synthesized in an Ar and N₂ mixture atmosphere by the bi-target reactive magnetron sputtering method. These films’ composition, microstructure and mechanical properties were characterized by energy dispersive spectroscopy, X-ray diffraction, scanning electron microscopy, atomic force microscopy and nanoindentation. Experimental results revealed that after the addition of silicon, Si₃N₄ interfacial phase formed on the surface of ZrN grains and prevented them from growing up. Zr-Si-N composite films were strengthened at low Si content with the hardness and elastic modulus reaching their maximum values of 29.8 and 352 GPa at 6.2 at% Si, respectively. With a further increase of Si content, the crystalline Zr-Si-N films gradually transformed into amorphous, accompanied with a remarkable fall of films’ mechanical properties. This limited enhancement of mechanical properties in the Zr-Si-N films may be due to the low wettability of Si₃N₄ on the surface of ZrN grains.     

Styrene-butadiene-glycidyl methacrylate terpolymer/silica composites: dispersion of silica particles and dynamic mechanical properties

Styrene-butadiene-glycidyl methacrylate terpolymer (GMA-SBR) was synthesized by emulsion polymerization for the fuel efficient tire tread composite. The chemical structure of the GMA-SBR was analyzed using infrared spectroscopy, ¹H NMR, gel permeation chromatography, and differential scanning calorimetry. The GMA-SBR/silica composite is the first instance introduced covalent bonds between silica filler and rubber molecules by in-chain modification of styrene-butadiene molecules. After compounding, the curing characteristics, the mechanical and dynamic mechanical properties of the composites were analyzed. The GMA-SBR/silica composite exhibited higher wear resistance of 32.9% and lower rolling resistance of 25.7% than the styrene-butadiene rubber 1721/silica composite. These results are due to the improvement of silica dispersion in the composite as the covalent bonding increased the filler–rubber interaction and the countervailing effects of less filler flocculation. The proposed approach assists in finding a solution to improve the performances of tires for fuel efficiency and the reduction of greenhouse gases from the vehicles.     

Tribological properties of chromium implanted silicon nitride ceramics correlated with microstructure

3 N₄ ceramic after chromium implantation were investigated for the dependence on implantation energy between 200 keV and 3 MeV at a fixed fluence of 10¹⁷ ions/cm². The wear of the modified material is reduced for a load of 2 N independent of ion energy accompanied by a slight increase of the friction coefficient. At higher loads only high-energy implantations result in improved wear behaviour. Structural investigations show the absence of any new phases formed by ion implantation. All energies result in an amorphous layer. For lower energies this amorphous layer reaches up to the surface whereas at higher energies it is covered by still-crystalline but damaged material. The observed wear behaviour can be explained with the amorphization of the near surface region and the stress generated by the volume swelling of the amorphous layer. Received: 25 November 1996/Accepted: 29 April 1997