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 Behavior of Fluorinated and Nonfluorinated Polyimide Films

In this study a series of polyimide (PI) films were synthesized from fluorinated and nonfluorinated monomers which contained diamines and dianhydrides. The influence of fluorine-containing groups on the glass transition temperature (T _g) and tribological properties of the PI films was investigated. The wear mechanism for the different kinds of PI polymers was comparatively discussed. T _g was characterized by dynamic mechanical analysis and the tribological changes were evaluated by friction and wear tests as well as scanning electron microscopy (SEM) analysis of the worn surfaces. Fourier transform infrared (FTIR) has been used to study the structures of the PI polymers. Experimental results indicated that the fluorine groups influenced the thermal behavior (T _g) of the PI films. Nonfluorinated PI films have lower friction coefficient and wear rate compared with the fluorinated ones. It was also found that the tribological properties of the PI films were closely related with the applied load. The friction coefficients and wear rates reduced with increasing the applied load.     

Tribological properties of chemically bonded polyimide films on silicon with polyglycidyl methacrylate brush as adhesive layer

Polyimide thin films, which possess good stability and film uniformity, are successfully fabricated on single crystal silicon wafers coated with a thin polymer brush by suface-initiated polymerization (SIP) as an adhesive layer. The growth kinetic of polyglycidyl methacrylate (PGMA) brush was studied by the means of ellipsometry. The nano-scale morphology and chemical composition of PGMA brush and polyimide film were studied with atomic force microscopy (AFM), Fourier transform infrared spectrum (FT-IR), and X-ray photoelectron spectroscopy (XPS). The tribological behaviors of the thin films sliding against AISI-52100 steel ball were examined on a static-dynamic friction precision measurement apparatus and UMT-2MT tribometer. The worn surface of the polyimide thin films was investigated with scanning electron microscopy (SEM). The results indicated that the chemically bonded polyimide films exhibited better friction reduction and antiwear behavior compared to the polymide films on bare silicon surface. At a load of 0.5 N and sliding speed of 20 mm s⁻¹, the durability life of the polyimide thin films is over 25,000 sliding cycles and the friction coefficient is about 0.08.     

A facile method for preparing highly conductive and reflective surface-silvered polyimide films

A novel method was developed for the preparation of reflective and electrically conductive surface-silvered polyimide (PI) films. The polyimide films were functionalized with poly(dopamine), simply by dipping the PI films into aqueous dopamine solution and mildly stirring at room temperature. Electroless plating of silver was readily carried out on the poly(dopamine) deposited PI (PI-DOPA) surface. The surface compositions of the modified PI films were studied by X-ray photoelectron spectroscopy (XPS). XPS results show that the PI-DOPA surfaces were successfully deposited with ploy(dopamine) and were ready for electroless deposition of silver. The poly(dopamine) layer was used not only as the chemi-sorption sites for silver particles during the electroless plating of silver, but also as an adhesion promotion layer for the electrolessly deposited silver. The as-prepared silvered PI films show high conductivity and reflectivity, with a surface resistance of 1.5 Ω and a reflectivity of 95%, respectively.     

Atomic oxygen erosion resistance of polyimide/ZrO2 hybrid films

A series of polyimide/zirconia (PI/ZrO₂) hybrid films were synthesized based on zirconium n-butoxide, pyromellitic acid dianhydride (PMDA) and 4,4′-oxydianiline (ODA) by a sol-gel process. The atomic oxygen (AO) exposure tests were carried out using a ground-based atomic oxygen effects simulation facility. The effects of ZrO₂ content on the morphology and structure evolvement of PI/ZrO₂ hybrid films were investigated using field emission scanning electron microscopy (FE-SEM) and X-ray photoelectron spectrometer (XPS), respectively. The results indicated that a zirconia-rich layer was formed on the polyimide film sourcing from the zirconium n-butoxide after AO exposure, which decreased the erosion rate and obviously improved the AO resistance of polyimide films.     

Origin of flat morphology and high crystallinity of ultrathin bismuth films

We have investigated the origin of “atomically flat” and “single-crystalline” growth of Bi films on Si(1 1 1)-7 × 7 through comparative experiments using Si(1 1 1)-β-√3 × √3-Bi as a control system. On the Si(1 1 1)-7 × 7 substrate, the majority of initial nuclei stabilize with pseudocubic (PC) paired layers analogous to the black phosphorus (BP) structure, and grow in a strong two-dimensional fashion that results in a “textured” but “atomically flat” surface morphology. After the coalescence of the BP-like grains at a nominal thickness of 4 monolayers (ML), a tiny number of minority hexagonal (HEX) bulk crystal nuclei, aligned commensurately with the substrate 7 × 7 lattice, cause the “textured” BP-like PC film to transform into a “single-crystalline” bulk-like HEX film. On the Si(1 1 1)-β-√3 × √3-Bi substrate, however, the BP-like structure breaks up into a conventional bulk-like PC structure and the HEX nucleation is suppressed up to as thick as ∼6 ML. Therefore, the morphology and crystallinity of the films are simply rough and polycrystalline, respectively.     

The effect of electro-annealing on the electrical properties of ITO film on colorless polyimide substrate

The effect of different annealing methods on the sheet resistance of indium tin oxide (ITO) on polyimide (PI) substrate has been investigated. ITO thin films were prepared by RF magnetron sputtering in pure Ar gas and electro-annealing, this was carried out in the flow of an electric current at several temperatures between 100 and 180 °C in air. Electro- and thermal annealing were compared in order to confirm differences between the electrical, optical and microstructural properties of the ITO thin films. As electro-annealing induced the predominant growth of crystallites of ITO thin films along (4 0 0) plane, the sheet resistance of ITO films that were electro-annealed for 2 mA at 180 °C considerably decreased from 50 to 28 Ω/cm².     

Micro- to nanoscale surface morphology and friction response of tribological polyimide surfaces

Sintered polyimide surfaces that were worn under macroscale conditions at different temperatures, were further characterised by contact-mode atomic force microscopy for getting insight in the tribophysical and -chemical processes at the micro- to nanoscale. Depending on the temperature, either mechanical interaction (23 °C < T < 100 °C), hydrolysis (120 °C < T < 140 °C), or imidisation (180 °C < T < 260 °C) results in different microscale surface characteristics. At low temperatures, surface brittleness and inter-grain fracture has been observed with an almost homogeneous friction pattern. At intermediate temperatures, the formation of a protecting local film leads to smoother surfaces with local lubricating properties. At high temperatures, different topographical and frictional patterns are observed depending on local imidisation or degradation. From AFM scans at the sub-micronscale, local debris depositions are observed and correspond to surface locations with locally reduced friction. From AFM scans at the nanoscale, polymer chain orientation is observed with formation of zig-zag or stretched molecular conformation: the latter is not induced by purely mechanical surface interactions or hydrolysis, but mainly results from tribochemically induced imidisation at high sliding temperatures. The present investigation describes the influences of local tribological interactions onto the macroscale wear behaviour of a polymer, and therefore aims at contributing to a better understanding of scaling between macro- to nanolevel tribological response.     

Bio-inspired dual surface modification to improve tribological properties at small-scale

In miniaturized devices like micro/nano-electro-mechanical systems (MEMS/NEMS), the critical forces, namely adhesion and friction restrict the smooth operation of the elements that are in relative motion. MEMS/NEMS are traditionally made of silicon, whose tribological properties are not good. In this paper, we present an investigation on the approach of dual surface modification of silicon surfaces and their tribological properties at micro-scale. The dual surface modification is a combination of topographical and chemical modifications. As the topographical modification, micro-patterns with varying shapes of pillars and channels were fabricated on Si(1 0 0) wafer surfaces using photolithography method. Chemical modification included the coating of micro-patterns with diamond-like carbon (DLC) and Z-DOL (perfluoropolyether, PFPE) thin films. The surfaces with combined modification were evaluated for their micro-friction behavior in comparison with those of bare Si(1 0 0) flat surfaces and the topographically/chemically modified silicon surfaces. Results showed that the surfaces with dual modification exhibited superior tribological properties. These results indicate that a combination of topographical and chemical modification is very effective in enhancing tribological properties at small-scale. The combined surface treatments such as the ones investigated in the current work could be useful for tribological applications in small-scale devices such as MEMS/NEMS. The motivation for undertaking the dual modification approach comes from an earlier observation made on the significant influence of the surface characteristics of lotus leaf on its micro-friction behavior.     

In situ Video-STM study of the potential-induced (1 × 1) → “hex” transition on Au(1 0 0) electrode surfaces in Cl containing solution

The potential-induced (1 × 1) → “hex” transition on Au(1 0 0) electrodes in 0.01 M Na₂SO₄ + 1 mM HCl was studied by in situ scanning tunneling microscopy at high time resolution (Video-STM). According to these observations the elementary units of the “hex” surface reconstruction, hexagonally-ordered strings in the Au surface layer, are highly dynamic nanoscale objects. Isolated “hex” strings exhibit dynamic fluctuations in structure and position on the millisecond timescale. These fluctuations exceed the mobility of multistring “hex” domains by several orders of magnitude and can be explained by collective dynamic processes within the strings. Furthermore, the observations reveal a novel 1D mass transport mechanism along the strings, details on the nucleation and growth of “hex” strings and complex string restructuring processes, facilitating “hex” domain ripening.     

Effect of surface property of polyimide substrate on the formation of pentacene thin-film

We investigated the effect of surface property of polyimide substrate on the formation of pentacene thin-film by using atomic force microscopy (AFM) and X-ray reflectivity (XRR) and diffuse scattering (XDS). Two types of polymer films were prepared: (1) polyimide (PAA-PI) from poly(amic acid) (PAA) (2) polyimide hybrid (PAA-PI-H) prepared by hybridizing the PAA and soluble polyimide (PI) with a octadecyl side chain. The hybridization ratio of PI to PAA was 2/98 in wt%. The water contact angle for PAA-PI-H and PAA-PI were around 80° and 64°, respectively. Morphology of pentacene with a ropelike structure and (1 1 0) peak around 1.4 Å in q_z was found when it was deposited on PAA-PI thin-film. Different pentacene morphology was observed when it was deposited on PAA-PI-H thin-film. The different morphology might be due to a 5-6 nm thick additional layer (∼0.95 ρ_film) at the interface between pentacene and PAA-PI-H thin-film caused by a long alkyl side chain introduced to the polymer main chain.     

Nanocrystalline nickel films with lotus leaf texture for superhydrophobic and low friction surfaces

Nanostructured Ni films with high hardness, high hydrophobicity and low coefficient of friction (COF) were fabricated. The surface texture of lotus leaf was replicated using a cellulose acetate film, on which a nanocrystalline (NC) Ni coating with a grain size of 30 ± 4 nm was electrodeposited to obtain a self-sustaining film with a hardness of 4.42 GPa. The surface texture of the NC Ni obtained in this way featured a high density (4 × 10³ mm⁻²) of conical protuberances with an average height of 10.0 ± 2.0 μm and a tip radius of 2.5 ± 0.5 μm. This structure increased the water repellency and reduced the COF, compared to smooth NC Ni surfaces. The application of a short-duration (120 s) electrodeposition process that deposited “Ni crowns” with a larger radius of 6.0 ± 0.5 μm on the protuberances, followed by a perfluoropolyether (PFPE) solution treatment succeeded in producing a surface texture consisting of nanotextured protuberances that resulted in a very high water contact angle of 156°, comparable to that of the superhydrophobic lotus leaf. Additionally, the microscale protuberances eliminated the initial high COF peaks observed when smooth NC Ni films were tested, and the PFPE treatment resulted in a 60% reduction in the steady-state COFs.     

Two routes to polycrystalline CoSi2 thin films by co-sputtering Co and Si

Two processes for the fabrication of polycrystalline CoSi₂ thin films based on the codeposition of Co and Si by sputtering were studied and compared. The first process involved “annealing after deposition”, where Co and Si are codeposited at ambient temperature and then crystallized by annealing. This process yielded randomly oriented plate-like CoSi₂ grains with a grain size that is governed by the nanostructure of the as-deposited film. Polycrystalline CoSi₂ thin films were obtained at a process temperature of 170 °C, which was much lower than the annealing temperature of 500 °C needed for Co/Si bilayers. The second process involved “heating during deposition”, where Co and Si are codeposited on heated substrates. This process yielded CoSi₂ grains with a columnar structure, and the grain size and degree of (1 1 1) orientation are temperature dependent. The sheet resistance of the resulting films was determined by the preparation temperature regardless of the deposition process used, i.e. “annealing after deposition” or “heating during deposition”. Temperatures of 500 °C and higher were needed to achieve CoSi₂ resistivity of 40 μΩ cm or lower for both processes.     

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。     

Luminescence and structure of ZnO-ZnS thin films prepared by oxidation of ZnS films in air and water vapor

Effect of water vapor quantity at oxidation of undoped ZnS films on structural and luminescent properties of the obtained films was investigated. The films were deposited onto glass substrates by electron beam evaporation. ZnO-ZnS layers were prepared by thermal oxidization of ZnS films at 600 °C in dry or wet atmospheres. The films were characterized by X-ray diffraction, atomic force microscopy and photoluminescence spectroscopy. As-deposited ZnS films were sphalerite crystal structure. The “dry annealing” led to the ZnS phase transition from sphalerite to wurtzite structure and from ZnS to ZnO for a small fraction of the film. After the “wet annealing” the amount of ZnO phase with wurtzite structure growing along the 〈0 0 0 2〉 direction varied from 25% to 95% in dependence on the water vapor quantity. Photoluminescent spectrum at room temperature exhibits green emission with maximum at 2.4 eV. A strong influence of the water vapor on shape and intensity of the emission was observed. Photoluminescent spectra at 22 K consisted of two bands—high-energy band at 2.1-2.4 eV and low energy band at 1.7-1.8 eV. Location and intensity ratio depended on the preparation conditions.     

The study of ion mixed amorphous carbon films on single crystal silicon by C ion implantation

Amorphous-carbon (a-C) films were deposited on a single-crystal silicon substrate by vacuum vapor deposition system and these amorphous carbon films were implanted with 110 keV C⁺ at fluences of 1 × 10¹⁷ ions/cm². The effect of ion mixing on the surface morphology, friction behavior and adhesion strengths of amorphous carbon films was examined making use of atomic force microscopy (AFM), ball-on-disk reciprocating friction tester, nano-indentation system and scanning electron microscope (SEM). The changes in chemical composition and structure were investigated by using X-ray photoelectron spectroscopy (XPS). The results show that the anti-wear life and adhesion of amorphous carbon films on the Si substrates were significantly increased by C ion implantation. The SiC chemical bonding across the interface plays a key role in the increase of adhesion strength and the anti-wear life of amorphous carbon film. The friction and wear mechanisms of amorphous carbon film under dry friction condition were also discussed.     

Electroless plating of copper on polyimide films modified by surface-initiated atom-transfer radical polymerization of 4-vinylpyridine

Surface modification of polyimide (PI) films were first carried out by chloromethylation under mild conditions, followed by surface-initiated atom-transfer radical polymerization (ATRP) of 4-vinylpyridine (4VP) from the chloromethylated PI surfaces. The composition and topography of the PI surfaces modified by poly(4-vinylpyridine) (P4VP) were characterized by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), respectively. The P4VP brushes with well-preserved pyridine groups on the PI surface was used not only as the chemisorption sites for the palladium complexes without prior sensitization by SnCl₂ solution during the electroless plating of copper, but also as an adhesion promotion layer to enhance the adhesion of the electrolessly deposited copper to the PI surfaces. The T-peel adhesion strength of the electrolessly deposited copper on the modified PI surface could reach about 6.6 N/cm. Effects of the polymerization time and the activation time in the PdCl₂ solution on the T-peel adhesion strength of the electrolessly deposited copper in the Sn-free process to the modified PI surface were also studied.     

An XPS study on ion beam induced oxidation of titanium silicide

Titanium silicides (TiSi₂) films grown on Si(1 0 0) substrate were investigated by ex situ XPS depth profiling after athermal ion beam induced oxidation (IBO) at 12 keV O₂⁺ incident energy and normal incidence. The composition and stoichiometry of these films were quantitatively determined as chemical state relative concentrations versus sputter time. “In depth” silicon and titanium oxidation states have been obtained after spectra deconvolution, showing a mixture of silicon dioxide, titanium dioxide, titanium suboxides, elemental titanium and residual traces of titanium nitride. Thermochemical data based on the corresponding enthalpies of formation of the oxides cannot explain our experimental results as in the case of low energy IBO, an oxygen defective altered layer is formed, presenting features of a reduced TiO_x phase.     

Structural and Tribological Properties of Polyimide/Al2O3/SiO2 Composites in Atomic Oxygen Environment

Effects of atomic oxygen (AO) irradiation on the structural and tribological behaviors of polyimide/Al₂O₃/SiO₂ composites were investigated in a ground-based simulation facility, in which the energy of AO was about 5 eV and the flux was 7.2 × 10¹⁵ cm^?2.s^?1. The structural changes were characterized by X-ray photoelectron spectroscopy (XPS) and attenuated total-reflection FTIR (FTIR-ATR), while the tribological changes were evaluated by friction and wear tests as well as scanning electron microscopy (SEM) analysis of the worn surfaces. It was found that AO irradiation induced the oxidation and degradation of polyimide (PI) molecular chains. The destructive action of AO changed the surface chemical structure, which resulted in changes of the surface morphology and chemical composition of the samples. Friction and wear tests indicated that AO irradiation decreased the friction coefficient but increased the wear rate of both pure and Al₂O₃/SiO₂ filled PIs.     

The photocatalytic application and regeneration of anatase thin films with embedded commercial TiO2 particles deposited on glass microrods

Anatase thin films (<200 nm in thickness) embedding Degussa P25 TiO₂ were prepared by sol-gel method. TiO₂-anatase thin films were deposited on a fiberglass substrate and then ground to obtain glass microrods containing the composite films. The film structure was characterized using Raman spectroscopy, atomic absorption and UV-vis spectrophotometry, and atomic force microscopy. The photocatalytic activity of the composite films, calcined at 450 °C, and the regeneration of the activity under the same experimental conditions, were assessed using gas chromatography to study the photodegradation of phenol, an industrial pollutant, in water under 365 nm irradiation. The film with 15.0 wt.% of P25 TiO₂ was found to be more photoactive (54 ppm of degraded phenol at 6 h of illumination) than the other ones.