Low Pressure Hexamethyldisiloxane (HMDSO)/Nitrogen Plasma Treatment on the Wettability and Surface Free Energy of Biaxial-Oriented Polypropylene (BOPP) Films

In this paper the influence of DC glow discharge HMDSO-N₂ plasma on wettability and surface properties of Biaxial-oriented polypropylene (BOPP) polymeric surfaces, has been investigated. The effects of plasma exposure time and HMDSO percent on the surface energy and wettability of the BOPP films were characterized using Fourier transform infrared spectroscopy (FTIR), Atomic force microscopy (AFM) and contact angle measurement. A clear change in the surface energy of BOPP films due to plasma treatment was observed. In this work we report changing surface properties of BOPP films instead of plasma treatment time and HMDSO ratios.     

Argon plasma irradiation of polypropylene

Polypropylene samples were exposed to argon plasma discharge and the changes of the PP surface properties were studied by different methods. Surface wettability was derived from contact angle measured by standard goniometry and chemical structure of the plasma modified PP was studied using X-ray photoelectron spectroscopy (XPS) and by Rutherford backscattering spectroscopy (RBS), surface morphology and roughness of samples using AFM. Zeta potential of pristine and modified PP was determined with the SurPASS. The presence of incorporated oxygen in the PP surface layer, about 60 nm thick, was observed in RBS spectra. Oxygen concentration is a decreasing function of the depth. With progressing aging time the oxygen concentration on the PP surface decreases. Plasma treatment results in a rapid decrease of the contact angle, which increases again with increasing aging time. In XPS measurement the oxygen containing structures, created by the plasma treatment, were found on the very surface of the modified PP and the zeta potential being changed too. The significant difference in zeta potential between pristine and plasma treated PP clearly indicates that the plasma treatment leads to a more hydrophilic PP surface.     

Influence of Chemical Precleaning on the Plasma Treatment Efficiency of Aluminum by RF Plasma Pencil

This paper is aimed to show the influence of initial chemical pretreatment prior to subsequent plasma activation of aluminum surfaces.The results of our study showed that the state of the topmost surface layer（i.e.the surface morphology and chemical groups）of plasma modified aluminum significantly depends on the chemical precleaning.Commonly used chemicals（isopropanol,trichlorethane,solution of Na OH in deionized water）were used as precleaning agents.The plasma treatments were done using a radio frequency driven atmospheric pressure plasma pencil developed at Masaryk University,which operates in Ar,Ar/O₂ gas mixtures.The effectiveness of the plasma treatment was estimated by the wettability measurements,showing high wettability improvement already after 0.3 s treatment.The effects of surface cleaning（hydrocarbon removal）,surface oxidation and activation（generation of OH groups）were estimated using infrared spectroscopy.The changes in the surface morphology were measured using scanning electron microscopy.Optical emission spectroscopy measurements in the near-to-surface region with temperature calculations showed that plasma itself depends on the sample precleaning procedure.     

Deposition of organosilicone thin film from hexamethyldisiloxane (HMDSO) with 50kHz/33MHz dual-frequency atmospheric-pressure plasma jet

The deposition of organosilicone thin films from hexamethyldisiloxane(HMDSO) by using a dual-frequency (50 kHz/33 MHz) atmospheric-pressure micro-plasma jet with an admixture of a small volume of HMDSO and Ar was investigated.The topography was measured by using scanning electron microscopy.The chemical bond and composition of these films were analyzed by Fourier transform infrared spectroscopy (FTIR) and x-ray photoelectron spectroscopy.The results indicated that the as-deposited film was constituted by silicon,carbon,and oxygen elements,and FTIR suggested the films are organosilicon with the organic component (-CHx) and hydroxyl functional group(-OH) connected to the Si-O-Si backbone.Thin-film hardness was recorded by an MH-5-VM Digital Micro-Hardness Tester.Radio frequency power had a strong impact on film hardness and the hardness increased with increasing power.     

Investigation of Microwave Surface-Wave Plasma Deposited SiOxCoatings on Polymeric Substrates简

In this paper, we reported nano-scale SiOx coatings deposited on polyethylene terephthalate （PET） webs by microwave surface-wave assisted plasma enhanced chemical vapor deposition for the purpose of improving their barrier properties. Oxygen （O2） and hexamethyl- disiloxane （HMDSO） were employed as oxidant gas and Si monomer during SiOx deposition, re- spectively. Analysis by Fourier transform infrared spectroscope （FTIR） for chemical structure and observation by atomic force microscopy （AFM） for surface morphology of SiO~ coatings demon- strated that both chemical compounds and surface feature of coatings have a remarkable influence on the coating barrier properties. It is noted that the processing parameters play a critical role in the barrier properties of coatings. After optimization of the SiOx coatings deposition conditions, i.e. the discharge power of 1500 W, 2 ： 1 of O2 ： HMDSO ratio and working pressure of 20 Pa, a better barrier property was achieved in this work.     

Cytocompatibility of Ar plasma treated and Au nanoparticle-grafted PE

Polyethylene (PE) was irradiated with inert Ar plasma, and the chemically active PE surface was grafted with Au nanoparticles. The composition and the structure of the modified PE surface were studied using X-ray photoelectron spectroscopy (XPS) and Rutherford backscattering spectroscopy (RBS). Changes in the surface wettability were determined from the contact angle measured in a reflection goniometer. The changes in the surface roughness and morphology were followed by atomic force microscopy (AFM). The modified PE samples were seeded with rat vascular smooth muscle cells (VSMC) or mouse NIH 3T3 fibroblasts, and their adhesion and proliferation were studied. We found that plasma discharge and Au grafting lead to dramatic changes in the surface morphology and roughness of PE. The Au nanoparticles were found not only on the sample surface, but also in the sample interior up to the depth of about 100 nm. In addition, plasma modification of the PE surface, followed with grafting Au-nanoparticles, significantly increased the attractiveness of the PE surface for the adhesion and growth of VSMC, and particularly for mouse embryonic 3T3 fibroblasts.     

Comparison of glow argon plasma-induced surface changes of thermoplastic polymers

Modification of high-density polyethylene (PE), polytetrafluoroethylene (PTFE), polystyrene (PS), polyethyleneterephthalate (PET) and polypropylene (PP) by Ar plasma was studied. The amount of the ablated material was determined by gravimetry. Wettability of polymers after the plasma treatment was determined from the contact angle measurement. The changes in the surface morphology of polymers were observed using atomic force microscopy (AFM). Chemical structure of modified polymers was characterized by X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR). Surface changes were also studied by the determination of electrokinetic potential (ζ-potential). It was found that under the plasma treatment the polymers are ablated and their surface morphology and roughness are changed dramatically. XPS measurements indicate an oxidation of the polymer surface. The plasma treatment results in a dramatic increase of the ζ-potential. EPR data show different radical amount present on the treated surface of all polymers. Most significant changes due to the degradation of polymer chains are observed on PTFE.     

Surface XPS-investigations of tobacco leaves treated with low-temperature plasma

The tobacco leaves were treated with low-temperature plasma in Ar, N2, O2. and air atmospheres at different powers （60-130 W）. The surface-elemental components, their relative contents, and the functional groups of the surface components of the tobacco leaves were determined using XPS （X-ray photoelectron spectroscopy）. The experimental results showed that the percentage of the elements C, N, and O had changed considerably and a large number of polar functional groups containing oxygen atoms were incorporated into the components on the tobacco surfaces. The measurements of the surface contact angle showed that the surface contact angle of the modified tobacco leaves was 0 degree, whereas it was 110 degrees before the plasma treatment. These results indicate that the wettability of the modified tobacco leaves improved dramatically. This work may be significant for future researches on the surface modification of the tobacco leaves.     

Formation of SiC Nanostruture Using Hexamethyldisiloxane During Plasma-Assisted Hot-Filament Chemical Vapor Deposition

Growth of SiC nanowires in plasma-assisted hot filament chemical-vapor-deposition by using hexamethyldisiloxane (HMDSO) as the gas source is reported. The SiC nanowires (SiCNWs) grew on Au-coated silicon substrate with Core-Shell structure, where the cores consisted of polycrystalline SiC grains and the shell exhibited amorphous structure. The featured structures such as cones, polyhedrons, ball-liked particles were observed in the case without plasma assistance. The underlying mechanism for the growth of nanostructures was also discussed. The high chemical activity induced by the plasma process plays an important role in using monomer to generate nanostructure.     

甲酸铈煅烧制备二氧化铈北大核心CSCD

以硝酸亚铈与甲酸反应后的甲酸铈为煅烧原料,在不同条件下煅烧后进行表征,分析煅烧产物的粒径、比表面积、形貌、碳含量、氮含量和氧与铈原子比(简称O/Ce比)。结果表明,煅烧后的颗粒粒径和形貌与煅烧前的颗粒粒径和形貌有关。16 mol/L甲酸与硝酸亚铈反应制备的甲酸铈颗粒煅烧前为棒状结构的团聚体,煅烧后形貌不变,粒径稍有减少,在煅烧温度高于700℃时产生大量粒径小于0.100μm细颗粒;而20 mol/L甲酸与硝酸亚铈反应制备的甲酸铈颗粒煅烧前为接近球体的团聚体,煅烧后形貌不变,但煅烧后即产生大量粒径小于0.100μm细颗粒。比表面积的降低是由孔结构减少引起的,随着煅烧温度的升高,晶体结构重新排列,晶格内缺陷减少,造成孔结构不断减少。煅烧后颗粒的碳含量和氮含量主要与煅烧温度有关,升高煅烧温度能有效降低碳含量和氮含量,而煅烧时间对碳含量和氮含量的影响较小。二氧化铈的晶体结构稳定,O/Ce比基本上维持在2.000±0.010之间。两种甲酸铈的煅烧工艺均选择煅烧温度为700℃,煅烧时间为1 h,煅烧时需要通入足量空气或氧气。     

Surface Sulfonation of Polyvinyl Chloride by Plasma for Antithrombogenicity

To enhance the blood compatibility of Polyvinyl Chloride (PVC) film, the film was modified by SO2/O2 gas plasma treatment. The effect of surface sulfonation of PVC treated by various SO2/O2 gas plasma depended on the volume ratio O2/(SO2 O2). When the volume ratio was 0.5, the effect of sulfonation was the best. Sulfonic acid groups were specifically and efficiently introduced onto the PVC surface, which was proved by X-ray photoelectron spectroscopy (XPS) and Attenuated Total Reflectance Fourier Transfer Infrared (ATR-FTIR) spectroscopy. The surface microstructure of modified PVC film was studied with scanning electron microscopy (SEM). The antithrombogenicity of the samples was determined by the activated partial thromboplastin time (APTT), prothrombin time (PT), thrombin time (TT) and plasma recalcification time (PRT) tests and platelet adhesion experiment. The results indicated that the antithrombogenicity of modified PVC was improved remarkably.     

Study on deposition of Al2O3 films by plasma-assisted atomic layer with different plasma sources

In this paper,A12O3 thin films are deposited on a hydrogen-terminated Si substrate by using two home-built electron cyclotron resonance (ECR) and magnetic field enhanced radio frequency plasma-assisted atomic layer deposition (PA-ALD) devices with Al(CH3)3 (trimethylaluminum,TMA) and oxygen plasma used as precursor and oxidant,respectively.The thickness,chemical composition,surface morphology and group reactions are characterized by in situ spectroscopic ellipsometer,x-ray photoelectric spectroscopy,atomic force microscopy,scanning electron microscopy,a high-resolution transmission electron microscope and in situ mass spectrometry (MS),respectively.We obtain that both ECR PA-ALD and the magnetic field enhanced PA-ALD can deposit thin films with high density,high purity,and uniformity at a high deposition rate.MS analysis reveals that the A12O3 deposition reactions are not simple reactions between TMA and oxygen plasma to produce alumina,water and carbon dioxide.In fact,acetylene,carbon monoxide and some other by-products also appear in the exhaustion gas.In addition,the presence of bias voltage has a certain effect on the deposition rate and surface morphology of films,which may be attributed to the presence of bias voltage controlling the plasma energy and density.We conclude that both plasma sources have a different deposition mechanism,which is much more complicated than expected.     

Plasma assisted synthesis of hollow nanofibers using electrospun sacrificial templates

In this work, we describe the synthesis of nanostructured polymeric materials of controlled tubular geometries using oxygen plasma and polysiloxane-grafting onto electrospun fiber sacrificial templates. The fibers were characterized using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) to determine the extent of grafting, graft chemistry and the influence of plasma treatment. Scanning electron microscopy (SEM) was used to determine the morphology and size of the electrospun fibers and nanotubes. The average diameter of the electrospun fibers employed ranged between 300 nm and 1500 nm. The micrographs revealed differences that are dependent on the type of grafting chemistry as well as plasma treatment times. The template synthesis of polysiloxane nanotubes using polyester track-etched membranes also shows that the technique is applicable to different substrates.     

Characteristics of Coaxial Dielectric Barrier Discharge at an Atmospheric Pressure with a Swirling Gas Argon/Oxygen Mixture for the Surface Modification of Polyester Fiber Cord

A newly developed coaxial dielectric barrier discharge reactor with a length of 1000 mm at an atmospheric pressure was used for plasma treatment of polyester fiber cord in a roll-to-roll manner. In this reactor, swirling mixture gases of oxygen of about 1% and argon with a flow rate of 1.5 to 2.7 L/min ensured the gas usage sparing, discharge uniformity and efficient fiber surface modification. The water contact angle and surface morphology of the treated fiber were measured. The results show that the surface oxygenation is mainly responsible for the wettability improvement of the fiber cord when passing through the plasma zone at a linear speed of 3 to 8 m/min. The specimens of modified-polyester fiber reinforced rubber composite were also prepared for the interfacial shear strength tests. Furthermore, the effect of adding oxygen into argon discharge on the fiber surface oxidation was correlated with optical emission spectroscopy. Finally, the effect of adding oxygen into argon discharge on the kinetic processes of the active species generation were also analyzed.     

Cleaning of nitrogen-containing carbon contamination by atmospheric pressure plasma jet

Atmospheric pressure plasma jet (APPJ) was used to clean nitrogen-containing carbon films (C–N) fabricated by plasma-assisted chemical vapor deposition method employing the plasma surface interaction linear device at Sichuan University (SCU-PSI). The properties of the contaminated films on the surface of pristine and He-plasma pre-irradiated tungsten matrix, such as morphology, crystalline structure, element composition and chemical structure were characterized by scanning electron microscopy, grazing incidence x-ray diffraction and x-ray photoelectron spectroscopy. The experimental results revealed that the removal of C–N film with a thickness of tens of microns can be realized through APPJ cleaning regardless of the morphology of the substrates. Similar removal rates of 16.82 and 13.78 μm min−1 were obtained for C–N films deposited on a smooth pristine W surface and rough fuzz-covered W surface, respectively. This is a remarkable improvement in comparison to the traditional cleaning method. However, slight surface oxidation was found after APPJ cleaning, but the degree of oxidation was acceptable with an oxidation depth increase of only 3.15 nm. Optical emission spectroscopy analysis and mass spectrometry analysis showed that C–N contamination was mainly removed through chemical reaction with reactive oxygen species during APPJ treatment using air as the working gas. These results make APPJ cleaning a potentially effective method for the rapid removal of C–N films from the wall surfaces of fusion devices.     

Effect of Gas Sources on the Deposition of Nano-Crystalline Diamond Films Prepared by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond (NCD) films were deposited on silicon substrates by a microwave plasma enhanced chemical vapor deposition (MPCVD) reactor in C2H5OH/H2 and CH4/H2/O2 systems, respectively, with a constant ratio of carbon/hydrogen/oxygen. By means of atomic force microscopy (AFM) and X-ray diffraction (XRD), it was shown that the NCD films deposited in the C2H5OH/H2 system possesses more uniform surface than that deposited in the CH4/H2/O2 system. Results from micro-Raman spectroscopy revealed that the quality of the NCD films was different even though the plasmas in the two systems contain exactly the same proportion of elements. In order to explain this phenomenon, the bond energy of forming OH groups, energy distraction in plasma and the deposition process of NCD films were studied. The experimental results and discussion indicate that for a same ratio of carbon/hydrogen/oxygen, the C2H5OH/H2 plasma was beneficial to deposit high quality NCD films with smaller average grain size and lower surface roughness.     

Characteristics of poly(vinylidene difluoride) modified by plasma-based ion implantation

Surface modification of polymers using radiation effects has been studied in a variety of fields, such as gas barrier or biochemical applications. However, the mechanism of improvement or degradation of polymers induced by radiation has not been well understood. In this study, poly(vinylidene difluoride) (PVDF) of crystalline phase of II (alpha form) was modified by plasma-based ion implantation (PBII) to control its adsorption properties for protein. Helium ions with applied bias voltages ranging from ?1 to ?20 kV were irradiated to the PVDF substrate for one minute and protein adsorption properties on the modified PVDF substrates was evaluated by the Western blotting method. As a result, adsorption of PVDF decreased with increasing the applied bias voltage, whereas the modification with only plasma treatment did not cause a significant change in adsorption properties for protein. The PBII-induced decrease in adsorption can be used for monitoring or patterning the protein. In order to study the mechanism, chemical and physical properties of the modified surfaces were analyzed with X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR) in attenuated total reflection (ATR) mode. Contact angles on the modified surfaces were also measured and surface free energies were calculated by Owens–Wendt–Rabel–Kaeble method. The surface morphology observed AFM and SEM did not show a significant change after the modification but the concentration of fluorine decreased and the surface energy on the surface increased after the modification. The influential factors in adsorption properties of the modified PVDF for protein are discussed.     

Surface Treatment of Polypropylene Powders Using a Plasma Reactor with a Stirrer

A radio frequency argon plasma reactor with a stirrer was employed for the surface treatment of polypropylene (PP) powders. The changes in the superficial contact angle and the superficial composition of the un-treated and treated PP powders were analyzed by means of water contact angle (WCA) measurement, X-ray photoelectron spectroscopy (XPS) and attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). The water contact angle changed from the original value of 130.2° before plasma treatment to the value of 73.6° after treatment for 5 minutes. With the increase in plasma treating time, there were a decrease in the water contact angle and an increase in the content of oxygen containing polar functional groups (i.e., C-O, C=O and O-C=O). Both XPS and ATR-FTIR results indicated that the plasma treatment led to the formation of oxygen containing polar functional groups due to oxidation on the surface of the PP powders, and the trend of variation of the water contact angle with plasma treating time was related to the concentration of oxygen atom on the treated PP powders surface. Furthermore, the aging of the plasma-treated PP powders was investigated.     

Estimation of plasma parameters in the process of micro-scale powder plastic and characteristics of its products

The temperature and density of plasma jets were estimated with a Boltzmann plot and Stark broadening of Ar I (696.54 nm) lines by optical emission spectroscopy (OES) in the process of plasma plastic, and the morphology and microstructure of tungsten (W) powders were investigated by scanning electron microscope (SEM) and x-ray Diffraction (XRD), respectively. The results show that the assumption of local thermodynamic equilibrium (LTE) was invalid at the end of the plasma jets, and earlier than this after the injection of tungsten powder. The temperature and electron density of the plasma jets were up to about T=6797 K with Q_c=50 slpm and n_e=1.05×10¹⁶ cm⁻³ with Q_s=115 slpm at Z=60 mm, respectively, and both dropped rapidly with the injected tungsten powders of 20 μm. After the plasma plastic process, the spherical tungsten powders were prepared and there were some satellite particles on the surface of the spherical products. The tungsten powders were both composed of a single equilibrium α-W phase with a body centered cubic (bbc) crystal structure before and after plasma treatment.