Electron beam initiated grafting of methacryloxypropyl-trimethoxysilane to fused silica glass

The effect of electron beam pretreatment of fused silica glass upon its surface functional composition and possibility for subsequent immobilization of methacryloxypropyl-trimethoxysilane (MOPTMS) layer is studied using FTIR spectroscopy and adsorption of acid-base indicators. The content of Brensted acidic centers (silanol groups) on the irradiated fused silica surface is found to follow an “oscillatory” trend as function of the absorbed dose below 100 kGy at electron beam processing due to the alternating reactions of hydroxylation (probably as a result of Si-O-Si bond disruption and interaction with radiolyzed physically adsorbed water) and thermal dehydration/dehydroxylation at radiation heating. The best conditions for MOPTMS layer formation are based on the increased acidity of both silica surface (formation of acidic hydroxyls) and the reaction medium (MOPTMS deposition from acetic acid solution). The optimal value of absorbed dose at electron beam processing providing the highest efficiency of MOPTMS grafting is 50 kGy at accelerated electron energy 700 keV. Electron beam pretreatment of fused silica surface is shown to provide more efficient MOPTMS immobilization in comparison with conventional chemical and thermal grafting procedures. The obtained results are promising for the enhancement of the processes for the production of fused silica glass capillaries for electrochromatography and electrophoresis at the stage of an intermediate bifunctional layer formation required for the subsequent deposition of specific polymer coatings.     

Effect of UV lamp irradiation during oxidation of Zr/Pt/Si structure on electrical properties of Pt/ZrO2/Pt/Si structure

Metal-insulator-metal (MIM) capacitors were fabricated using ZrO₂ films and the effects of structural and native defects of the ZrO₂ films on the electrical and dielectric properties were investigated. For preparing ZrO₂ films, Zr films were deposited on Pt/Si substrates by ion beam deposition (IBD) system with/without substrate bias voltages and oxidized at 200 °C for 60 min under 0.1 MPa O₂ atmosphere with/without UV light irradiation (λ = 193 nm, Deep UV lamp). The ZrO₂(∼12 nm) films on Pt(∼100 nm)/Si were characterized by X-ray diffraction pattern (XRD), field emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HRTEM), capacitance-voltage (C-V) and current-voltage (I-V) measurements were carried out on MIM structures. ZrO₂ films, fabricated by oxidizing the Zr film deposited with substrate bias voltage under UV light irradiation, show the highest capacitance (784 pF) and the lowest leakage current density. The active oxygen species formed by UV irradiation are considered to play an important role in the reduction of the leakage current density, because they can reduce the density of oxygen vacancies.     

The sterilization of Escherichia coli by dielectric-barrier discharge plasma at atmospheric pressure

The sterilization of E. coli (ATCC8099) using an atmospheric pressure, air DBD plasma driven by 100 Hz high-voltage power supply was investigated in this paper. The results showed that germicidal efficiency was closely related to the plasma treatment time, the gap spacing, the initial cell density and the surface characters of substrate materials. The germicidal efficiency was 99.999% under the conditions of 5-min plasma treatment, 3-cm gap spacing and on PET films. After plasma exposure for 5 min, the temperature was observed below 43 °C which could not lead to inactivate E. coli. The observation of protein leakage and cell morphology alteration by transmission electron microscopy (TEM) techniques revealed that the etching action on cell membrane by electrons, ions and radicals was primary reason of DBD air plasma sterilization.     

Observation of regular defects formed on the surface of PbTe thin films grown by molecular beam epitaxy

Regular shape defects on the surface of PbTe thin films grown by molecular beam epitaxy (MBE) were studied by scanning electron microscope (SEM). Two types of regular shape defects were observed on Te-rich PbTe films grown at substrate temperature T ≥ 235 °C with a beam flux ratio of Te to PbTe (R_f) to be 0.5 and at 280 °C with a R_f ≥ 0.4, which include cuboids and triangular pyramids. The formation mechanism of the observed regular shape defects is interpreted as following: They are the outcome of fast growth rate along {1 0 0} crystal planes that have the lowest surface energy and the enclosure of the {1 0 0} crystal planes. The formation of the regular shape defects in the growth of PbTe needs appropriate substrate temperature and Te-rich ambience. However, when R_f is decreased low enough to make the films slightly Pb-rich, triangular pits that originate from the insufficient glide of the threading dislocations along the main 〈1 1 0〉 {1 0 0} glide system of PbTe in Cottrell atmosphere, will be the main feature on the film surface.     

Influence of substrate crystallography on the room temperature synthesis of AlN thin films by reactive sputtering

A pulsed DC reactive ion beam sputtering system has been used to synthesize aluminium nitride (AlN) thin films at room temperature by reactive sputtering. After systematic study of the processing variables, high-quality polycrystalline films with preferred c-axis orientation have been grown successfully on silicon and Au/Si substrates with an Al target under a N₂/(N₂ + Ar) gas flow ratio of 55%, 2 mTorr processing pressure and keeping the temperature of the substrate holder at room temperature. The crystalline quality of the AlN layer as well as the influence of the substrate crystallography on the AlN orientation has been characterized by high-resolution X-ray diffraction (HR-XRD). Best ω-FWHM (Full Width at Half Maximum) values of the (0 0 0 2) reflection rocking curve in the 1 μm thick AlN layers are 1.3°. Atomic Force Microscopy (AFM) measurements have been used to study the surface morphology of the AlN layer and Transmission Electron Microscopy (TEM) measurements to investigate the AlN/substrate interaction. AlN grew off-axis from the Si substrate but on-axis to the surface normal. When the AlN thin film is deposited on top of an Au layer, it grows along the [0 0 0 1] direction but showing a two-domain structure with two in-plane orientations rotated 30° between them.     

Formation of Pt-C films by ion beam assisted deposition for the application of suppression thermo-electron emission

Platinum and carbon were deposited onto the surface of molybdenum grids simultaneously by ion beam assisted deposition. The structure of the Pt-C films was studied by XRD and Raman spectroscopy. The XRD results showed that Pt exhibited mixed strong (1 1 1) and weak (2 0 0) orientations. The Raman spectra showed that the carbon existed in the form of graphite-like phase. Electron emission characteristics from the Mo grid with and without Pt-C films were measured using analogous diode method. The results showed that electron emission from the Mo grid coated with Pt-C films was much less than that from the Mo grid without Pt-C films. The obtained results demonstrated that the Pt-C films are effective grid-coating materials for the application of suppression thermo-electron emission.     

Observation of triangle pits in PbSe grown by molecular beam epitaxy

PbSe thin films on BaF₂ (1 1 1) were grown by molecular beam epitaxy with different selenium beam flux. Evolution of PbSe surface morphologies with Se/PbSe beam flux ratio (R_f) has been studied by atomic force microscopy and high-resolution X-ray diffraction. Growth spirals with monolayer steps on PbSe surface are obtained using high beam flux ratio, R_f ≥ 0.6. As R_f decreases to 0.3, nano-scale triangle pits are formed on the surface and the surface of PbSe film changes to 3D islands when R_f = 0. Glide of threading dislocations in 〈1 1 0〉{1 0 0}-glide system and Pb-rich atom agglomerations are the formation mechanism of spiral steps and triangle pits. The nano-scale triangle pits formed on PbSe surface may render potential applications in nano technology.     

Effects of evolving surface morphology on yield during focused ion beam milling of carbon

We investigate evolving surface morphology during focused ion beam bombardment of C and determine its effects on sputter yield over a large range of ion dose (10¹⁷-10¹⁹ ions/cm²) and incidence angles (Θ = 0-80°). Carbon bombarded by 20 keV Ga⁺ either retains a smooth sputtered surface or develops one of two rough surface morphologies (sinusoidal ripples or steps/terraces) depending on the angle of ion incidence. For conditions that lead to smooth sputter-eroded surfaces there is no change in yield with ion dose after erosion of the solid commences. However, for all conditions that lead to surface roughening we observe coarsening of morphology with increased ion dose and a concomitant decrease in yield. A decrease in yield occurs as surface ripples increase wavelength and, for large Θ, as step/terrace morphologies evolve. The yield also decreases with dose as rippled surfaces transition to have steps and terraces at Θ = 75°. Similar trends of decreasing yield are found for H₂O-assisted focused ion beam milling. The effects of changing surface morphology on yield are explained by the varying incidence angles exposed to the high-energy beam.     

Oxygen flux influence on the morphological, structural and optical properties of Zn1−xMgxO thin films grown by plasma-assisted molecular beam epitaxy

The Zn_1−xMg_xO thin films were grown on Al₂O₃ substrate with various O₂ flow rates by plasma-assisted molecular beam epitaxy (P-MBE). The growth conditions were optimized by the characterizations of morphology, structural and optical properties. The Mg content of the Zn_1−xMg_xO thin film increases monotonously with decreasing the oxygen flux. X-ray diffractometer (XRD) measurements show that all the thin films are preferred (0 0 2) orientated. By transmittance and absorption measurements, it was found that the band gap of the film decreases gradually with increasing oxygen flow rate. The surface morphology dependent on the oxygen flow rate was also studied by field emission scanning electron microscopy (FE-SEM). The surface roughness became significant with increasing oxygen flow rate, and the nanostructures were formed at the larger flow rate. The relationship between the morphology and the oxygen flow rate of Zn_1−xMg_xO films was discussed.     

Influence of deposition temperature on the crystallinity of Al-doped ZnO thin films at glass substrates prepared by RF magnetron sputtering method

Al-doped ZnO (AZO) transparent conducting films were successfully prepared on glass substrates by RF magnetron sputtering method under different substrate temperatures. The microstructural, electrical and optical properties of AZO films were investigated in a wide temperature range from room temperature up to 350 °C by X-ray Diffraction (XRD), Field-Emission Scanning Electron Microscopy (FESEM), High-Resolution Transmission Electron Microscopy (HRTEM), Hall measurement, and UV–visible meter. The nature of AZO films is polycrystalline thin films with hexagonal wurtzite structure and a preferred orientation along c-axis. The crystallinity and surface morphologies of the films are strongly dependent on the growth temperature, which in turn exerts a great effect on microstructural, electrical and optical properties of the AZO films. The atomic arrangement of AZO film having an wurtzite structure was indeed identified by the HRTEM as well as the Selected Area Electron Diffraction (SAED). The defect density of AZO film was investigated by HRTEM. The film deposited at 100 °C exhibited the relatively well crystallinity and the lowest resistivity of 3.6 × 10⁻⁴ Ω cm. The average transmission of AZO films in the visible range is all over 85%. More importantly, the low-resistance and high-transmittance AZO film was also prepared at a low temperature of 100 °C.     

Influence of assisted ion energy on surface roughness and mechanical properties of boron carbon nitride films synthesized by DIBSD

The BCN thin films were produced by dual ion beam sputtering deposition (DIBSD). The influence of assisted ion energy on surface roughness and mechanical properties of BCN films were investigated. The surface roughness was determined by atomic force microscopy (AFM) and the mechanical properties of BCN firms were evaluated by nano-indentation in N₂ gas. The composition, structure and chemical bonding of the BCN thin films were analyzed by using energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), laser Raman spectroscopy and Fourier transform infrared spectroscopy (FTIR). These films appeared as amorphous structure. As a result, the BCN films with the smoothest surface (R_a = 0.35 nm and R_p-v = 4.4 nm) and the highest nano-hardness of 30.1 GPa and elastic modulus of 232.6 GPa were obtained at 200 eV and 12 mA with N₂:Ar = 1:1, and the chemical composition of this BCN film was 81 at.% B, 14 at.% C and 5 at.% N. Moreover, several bonding states such as B-N, B-C and C-N were observed in BCN thin films.     

Ultra smooth NiO thin films on flexible plastic (PET) substrate at room temperature by RF magnetron sputtering and effect of oxygen partial pressure on their properties

Transparent p-type nickel oxide thin films were grown on polyethylene terephthalate (PET) and glass substrates by RF magnetron sputtering technique in argon + oxygen atmosphere with different oxygen partial pressures at room temperature. The morphology of the NiO thin films grown on PET and glass substrates was studied by atomic force microscope. The rms surface roughnesses of the films were in the range 0.63-0.65 nm. These ultra smooth nanocrystalline NiO thin films are useful for many applications. High resolution transmission electron microscopic studies revealed that the grains of NiO films on the highly flexible PET substrate were purely crystalline and spherical in shape with diameters 8-10 nm. XRD analysis also supported these results. NiO films grown on the PET substrates were found to have better crystalline quality with fewer defects than those on the glass substrates. The sheet resistances of the NiO films deposited on PET and glass substrates were not much different; having values 5.1 and 5.3 kΩ/□ and decreased to 3.05, 3.1 kΩ/□ respectively with increasing oxygen partial pressure. The thicknesses of the films on both substrates were ∼700 nm. It was also noted that further increase in oxygen partial pressure caused increase in resistivity due to formation of defects in NiO.     

Effects of l-arginine immobilization on the anticoagulant activity and hemolytic property of polyethylene terephthalate films

Surface modification of polyethylene terephthalate (PET) films was performed with l-arginine (l-Arg) to gain an improved anticoagulant surface. The surface chemistry changes of modified films were characterized by X-ray photoelectron spectroscopy (XPS) and attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. The in vitro anticoagulant activities of the surface-modified PET films were evaluated by blood clotting test, hemolytic test, and the measurement of clotting time including plasma recalcification time (PRT), activated partial thromboplastin time (APTT), and prothrombin time (PT). The data of blood coagulation index (BCI) for l-arginine modified PET films (PET-Arg) was larger than that for PET at the same blood-sample contact time. The hemolysis ratio for PET-Arg was less than that for PET and within the accepted standard for biomaterials. The PRT and APTT for PET-Arg were significantly prolonged by 189 s and 25 s, respectively, compared to those for the unmodified PET. All results suggested that the currently described modification method could be a possible candidate to create antithrombogenic PET surfaces which would be useful for further medical applications.     

Field emission measured from nanostructured germanium and silicon thin films

We have prepared nanostructured thin films of germanium and silicon. The films were grown by an ion beam sputtering technique followed by a rapid annealing step using an electron beam annealer. The annealing temperature is a comparatively low 500 °C, resulting in well defined nano-islands on the film surface. Electron field emission has been measured from the surfaces under high vacuum. The threshold electric field value for significant current flow was measured as 2.5 V μm⁻¹ for a silicon thin film which is comparable to other silicon technologies. A value of 0.5 V μm⁻¹ for a germanium thin film represents an order of magnitude improvement for related germanium nanostructured systems.     

AES, LEED and PYS investigation of Au deposits on InSe/Si(1 1 1) substrate

Auger Electron Spectroscopy (AES), Low Energy Electron Diffraction (LEED) and Photoelectron Yield Spectroscopy (PYS) measurements have been used to monitor the interaction of gold (Au) deposits on InSe/Si(1 1 1) substrate. Au has been sequentially deposed under ultra-high vacuum onto 40 Å-thick film of layered semiconductor InSe which is epitaxially grown by molecular beam epitaxy (MBE) on a Si(1 1 1)1 × 1-H substrate and kept at room temperature. Au coverage varies from 0.5 monolayer to 20 monolayers (ML) (in terms of InSe atomic surface plane: 1 ML = 7.2 1014 at/cm²) which is corresponding to 1.30 Å of Au-metal. The Au/InSe/Si(1 1 1) system was characterized as function of Au deposit, we noticed an interaction at room temperature starts as an apparent intercalation process until 5 ML. Beyond this dose Au islands begin to form on the sample surface without interaction with InSe substrate, thus the interface is far from to be a simple junction Au-InSe.     

Structural phase transitions in Au thin films on Si (1 1 0): An in situ temperature dependent transmission electron microscopy study

We present a review on the formation of gold silicide nanostructures using in situ temperature dependent transmission electron microscopy (TEM) measurements. Thin Au films of two thicknesses (2.0 nm and 5.0 nm) were deposited on Si (1 1 0) substrate under ultra-high vacuum (UHV) conditions in a molecular beam epitaxy (MBE) system. Also a 2.0 nm thick Au film was deposited under high vacuum condition (with the native oxide at the interface of Au and Si) using thermal evaporation. In situ TEM measurements (for planar samples) were made at various temperatures (from room temperature, RT to 950 °C). We show that, in the presence of native oxide (UHV-MBE) at the interface, high aspect ratio (≈15.0) aligned gold silicide nanorods were observed. For the films that were grown with UHV conditions, a small aspect ratio (∼1.38) nanogold silicide was observed. For 5.0 nm thick gold thin film, thicker and lesser aspect ratio silicides were observed. Selected area diffraction pattern taken at RT after the sample for the case of 5.0 nm Au on Si (1 1 0)-MBE was annealed at 475 °C show the signature of gold silicide formation.     

Biocompatible and bioactive nanostructured glass coatings synthesized by pulsed laser deposition: In vitro biological tests

We report on the synthesis by pulsed laser deposition with a KrF* excimer laser source (λ = 248 nm, τ = 25 ns) of bioglass thin films of 6P57 and 6P61 types. Physiology, viability, and proliferation of human osteoblast cells were determined by quantitative in vitro tests performed by flow cytometry on primary osteoblasts cultured on pulsed laser deposited bioglasses. Both types of glass films proved to be appropriate mediums for cell survival and proliferation. In a parallel investigation, cell morphology and adhesion to the surface was studied by fluorescence microscopy and scanning electron microscopy. Strong bonds between the materials and cells were found in both cases, as osteoblast pseudopodes penetrated deep into the material. According to our observations, the 6P57 glass films were superior with respect to viability and proliferation performances.     

Growth of cubic MgxZn1−xO alloy films by electron beam evaporation

We report the growth of cubic Mg_xZn_1−xO alloy thin films on quartz by electron beam evaporation. It can be found that all the samples have sharp absorption edges by the absorption measurements. X-ray diffraction measurements indicate the Mg_xZn_1−xO films are cubic phase with preferred orientation along the (1 1 1) direction. Energy dispersive spectrometry (EDS) demonstrates that the Mg concentration in Mg_xZn_1−xO films is much higher than the ceramic target used, and the composition can be tuned in a small scope by varying the substrate temperature and the beam electric current. The reasons of this phenomenon are also discussed.     

Structure and optical properties of ZnS thin films grown by glancing angle deposition

The glancing angle deposition (GLAD) technique was used to deposit ZnS films by electron beam evaporation method. The cross sectional scanning electron microscopy (SEM) image illustrated a highly orientated microstructure composed of slanted column. The atomic force microscopy (AFM) analysis indicated that incident flux angle had significant effects on the nodule size and surface roughness. Under identical nominal thickness, the actual thickness of the GLAD films is related to the incident flux angle. The refractive index and in-plane birefringence of the GLAD ZnS films were discussed, and the maximum birefringence Δn = 0.036 was obtained at incident flux angle of α = 80°. Therefore, the glancing angle deposition technique is a promising way to create a columnar structure with enhanced birefringent property.     

Effects of electron irradiation on the properties of GZO films deposited with RF magnetron sputtering

Transparent conductive GZO films were deposited on polycarbonate substrates by electron beam assisted radio frequency (RF) magnetron sputtering and then the influence of electron irradiation on the structural, optical and electrical properties of GZO films was investigated by using X-ray diffractometry, UV-vis spectrophotometry, four point probes, atomic force microscopy and UV photoelectron spectroscopy. Sputtering power was kept constant at 3 W/cm² during deposition, while electron irradiation energy varied from 450 to 900 eV.Electron irradiated GZO films show larger grain sizes than those of films prepared without electron irradiation, and films irradiated at 900 eV show higher optical transmittance in the visible wavelength region and lower sheet resistance (120 Ω/□) than other films. The work-function is also increased with electron irradiation energy. The highest work-function of 4.4 eV was observed in films that were electron irradiated at 900 eV.