Tarnish Testing of Copper-Based Alloys Coated with SiO_2-Like Films by PECVD

The tarnishing test in the presence of hydrogen sulfide（H2S） vapors has been used to investigate the tarnish resistance capability of copper-based alloys coated with Si02-like films by means of plasma-enhanced chemical vapor deposition（PECVD） fed with a tetraethoxysilane/oxygen mixture.The chemical and morphological properties of the films have been characterized by using infrared absorption spectroscopy（IR） and scanning electron microscopy（SEM）with energy disperse spectroscopy（EDS）.The corrosion products of the samples after the tarnishing test have been identified by X-ray diffraction analysis（XRD）.It has been found that SiO2-like films formed via PECVD with a high O2 flow rate could protect copper-based alloys from H2S vapor tarnishing.The alloys coated at the O2 flow rate of 20 sccm remain uncorroded after 54days of H2S vapor tarnish testing.The corrosion products for the alloys deposited at a low O2flow rate after 54 days of tarnish testing are mainly composed of brochantite.     

The Effect of Plasma Surface Treatment on a Porous Green Ceramic Film with Polymeric Binder Materials

To reduce time and energy during thermal binder removal in the ceramic process, plasma surface treatment was applied before the lamination process.The adhesion strength in the lamination films was enhanced by oxidative plasma treatment of the porous green ceramic film with polymeric binding materials.The oxygen plasma characteristics were investigated through experimental parameters and weight loss analysis.The experimental results revealed the need for parameter analysis,including gas material,process time,flow rate,and discharge power,and supported a mechanism consisting of competing ablation and deposition processes.The weight loss analysis was conducted for cyclic plasma treatment rather than continuous plasma treatment for the purpose of improving the film’s permeability by suppressing deposition of the ablated species.The cyclic plasma treatment improved the permeability compared to the continuous plasma treatment.     

An investigation on improving the homogeneity of plasma generated by linear microwave plasma source with a length of 1550 mm

To develop a larger in-line plasma enhanced chemical vapor deposition(PECVD) device, the length of the linear microwave plasma source needs to be increased to 1550 mm. This paper proposes a solution to the problem of plasma inhomogeneity caused by increasing device length.Based on the COMSOL Multiphysics, a multi-physics field coupling model for in-line PECVD device is developed and validated. The effects of microwave power, chamber pressure, and magnetic flux density on the plasma distribution are investigated, respectively, and their corresponding optimized values are obtained. This paper also presents a new strategy to optimize the wafer position to achieve the balance between deposition rate and film quality. Numerical results have indicated that increasing microwave power and magnetic flux density or decreasing chamber pressure all play positive roles in improving plasma homogeneity, and among them, the microwave power is the most decisive influencing factor. It is found that the plasma homogeneity is optimal under the condition of microwave power at 2000 W, chamber pressure at15 Pa, and magnetic field strength at 45 mT. The relative deviation is within-3.7% to 3.9%,which fully satisfies the process requirements of the equipment. The best position for the wafer is88 mm from the copper antenna. The results are very valuable for improving the quality of the in-line PECVD device.     

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.     

Effect of Low Pressure Nitrogen–Oxygen (N<Subscript>2</Subscript>/O<Subscript>2</Subscript>) Plasma Treatment on Surface Properties of Polypropylene Films

In this paper the effect of plasma treatment by using mixed gas (N₂/O₂) on surface properties of a Polypropylene PP films were investigated as a function of O₂ content and treatment time. Results obtained by using Fourier Transform infrared spectrometer (FTIR), contact angle measurement and scanning electron microscopy (SEM). It is found that plasma treatment can change chemical structure of polymer surfaces partially. SEM images revealed distinct changes in topography of PP due to O₂/N₂ plasma treatment. Finally wettability and surface energy before and after treatment investigated in different conditions.     

Characteristics of high deposition rate PIN diodes from pure SiH4 and 10% dilution of SiH4 in H2

In this paper, we present the results of the electrical characterization of PIN diodes up to 18 μm thick fabricated on high deposition rates a-Si:H layers obtained from pure SiH₄ and from a 10% dilution of SiH₄ in H₂, using a 13.56 MHz plasma enhanced chemical vapor deposition (PECVD) with geometrical modifications in the plasma reactor. I-V and I-T curves were investigated, concluding that the changes introduced in the deposition reactor to increase the deposition rate did not affect the characteristics of the fabricated diodes. Results are compared with characteristics, reported for diodes obtained by standard and other high deposition rate methods     

The effect of nitrogen concentration on the properties of N-DLC prepared by helicon wave plasma chemical vapor deposition

Nitrogen-doped diamond-like carbon (N-DLC) films were synthesized by helicon wave plasma chemical vapor deposition (HWP-CVD). The mechanism of the plasma influence on the N-DLC structure and properties was revealed by the diagnosis of plasma. The effects of nitrogen doping on the mechanical and hydrophobicity properties of DLC films were studied. The change in the ratio of precursor gas flow reduces the concentration of film-forming groups, resulting in a decrease of growth rate with increasing nitrogen flow rate. The morphology and structure of N-DLC films were characterized by scanning probe microscopy, Raman spectroscopy, and X-ray photoemission spectroscopy. The mechanical properties and wettability of N-DLC were analyzed by an ultra-micro hardness tester and JC2000DM system. The results show that the content ratio of N+ and ${{\rm{N}}}_{2}^{+}$ is positively correlated with the mechanical properties and wettability of N-DLC films. The enhancement hardness and elastic modulus of N-DLC are attributed to the increase in sp3 carbon–nitrogen bond content in the film, reaching 26.5 GPa and 160 GPa respectively. Water contact measurement shows that the increase in the nitrogen-bond structure in N-DLC gives the film excellent hydrophobic properties, and the optimal water contact angle reaches 111.2°. It is shown that HWP technology has unique advantages in the modulation of functional nanomaterials.     

316L不锈钢基材防氚渗透Al2O3涂层残余热应力分析

在聚变堆防氚渗透第一壁制备过程中,Al2O3涂层与316 L不锈钢基体间由于材料热膨胀系数的差异容易产生裂纹.本文利用有限元方法研究了AL2O3/316 L涂层制备过程中的残余应力的分布.结果表明在界面等区域存在严重的应力集中;涂层厚度、孔隙率大小以及涂层是否致密对残余应力水平有很大影响.涂层内部关键区域的残余应力水平,随着涂层厚度增加而增加;孔隙率不同对界面的残余应力分布趋势没有明显影响,但对应力值却有很大影响,孔隙率增大涂层残余应力最大值下降;相同厚度情况下致密Al2O3涂层所受压应力远大于多孔Al2O3涂层承受的残余应力.     

基于单一气源的PECVD方法制备SiC薄膜及其微观结构研究

为制备出满足惯性约束聚变（ICF）实验要求的SiC薄膜,本文采用等离子体增强化学气相沉积（PECVD）法,以四甲基硅（TMS）作为唯一反应气源,在不同工作压强下制备SiC薄膜。利用扫描电子显微镜、表面轮廓仪、原子力显微镜、精密电子天平、X射线光电子能谱、傅里叶变换红外光谱对薄膜进行表征与分析。结果表明：SiC薄膜的成分与工作压强密切相关,随着工作压强的增加,薄膜中Si含量整体呈下降趋势;随着工作压强的增加,薄膜沉积速率先增大后减少,密度先减小后增大;与其他制备工艺相比,采用单一气源制备SiC薄膜,其表面粗糙度极低（1.25～1.85 nm）,薄膜粗糙度随工作压强的增加呈先增大后减小的趋势。     

Preparation of a new micro-porous poly(methyl methacrylate)-grafted polyethylene separator for high performance Li secondary battery

In this study, micro-porous poly(methyl methacrylate)-grafted polyethylene separators (PE-g-PMMA) were prepared by a radiation-induced graft polymerization of methyl methacrylate onto a conventional PE separator followed by a phase inversion. After the phase inversion, the micro-pores were generated in the grafted PMMA layer. The prepared micro-porous PE-g-PMMA separators showed an improved electrolyte uptake and ionic conductivity due to their improved affinity with a liquid electrolyte and the presence of pores in the grafted PMMA layer. The PE-g-PMMA separators exhibited a lower thermal shrinkage compared to the original PE separator. The PE-g-PMMA separators showed a better oxidation stability up to 5.0 V when compared to the original PE separator (4.5 V).     

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.     

Atmospheric Pressure Plasma Jet in Ar and O2/Ar Mixtures： Properties and High Performance for Surface Cleaning＊

An atmospheric pressure plasma jet generated in Ar and O2/Ar mixtures has been investigated by specially designed equipment with double power electrodes at 20~32 kHz, and their effects on the cleaning of surfaces have been studied. Properties of the jet discharge are studied by electrical diagnostics, including the waveform of discharge voltage, discharge current and the Q-V Lissajous figures. The optical emission spectroscopy is used to measure the plasma parameters, such as the excitation temperature and the gas temperature. It is found that the consumed power and the excitation temperature increase with increase of the discharge frequency. On the other hand, at the same discharge frequency, these parameters in O2/Ar mixture plasma are found to be much larger. The effect on surface cleaning is studied from the changes in the contact angle. For Ar plasma jet, the contact angle decreases with increase of the discharge frequency. For O2/Ar mixture plasma jet, the contact angle decreases with increase of discharge frequency up to 26 kHz, however, further increase of discharge frequency does not show further decrease in the contact angle. At the same discharge frequency, the contact angle after O2/Ar mixture plasma cleaning is found to be much lower compared to the case of pure Ar. From the results of quadrupole mass-spectrum analysis, we can identify more fragment molecules of CO and H2O in the emitted gases after O2/Ar plasma jet treatment compared with Ar plasma jet treatment, which are produced by the decomposition of surface organic contaminants during the cleaning process.     

Study of polypropylene/polybutene blends modified by gamma irradiation and (high melt strength polypropylene)/polybutene blends

It is well-known that polypropylene (PP) is difficult to process as a consequence of its linear structure. It is also known that grafting of long-chain branches on PP backbone using ionizing radiation is an effective approach to achieve high melt strength polypropylene (HMS PP). Chain-scission and, in minor extend, crosslinking and grafting are the predominant reaction in order to branch PP backbone. However, if multifunctional monomers are used to promote the grafting reaction, crosslinking can surpass chain scission and grafting, reducing drawability. Therefore, in an effort to enhance the processability and so the drawability, it has been found helpful to add a small amount of polybutene-1. Gamma irradiation technique was used to induce chemical changes in blends of PP and polybutene in acetylene atmosphere (crosslinker promoter) and in HMSPP/polybutene blends. The samples were irradiated with a ⁶⁰Co source with doses of 12.5 and 20 kGy in the presence of acetylene. In this work, two different methods of blends processing were compared regarding rheological and mechanical properties. Effects on the strength and elongation at the yield point and at rupture were observed by mechanical tests and showed decrease of tensile strength and increase of elongation at rupture for samples obtained by irradiation of blends. The results from rheology demonstrated an increase in melt strength and drawability of blends.     

In vitro study of nonthermal atmospheric pressure plasma in improving the durability of the dentin–adhesive interface with an etch-and-rinse system

In this study, we employed a nonthermal atmospheric pressure plasma (NTAPP) jet to evaluate the effect of plasma treatment on the durability of resin–dentin bonding under a thermocycling challenge. Furthermore, we assessed the degradation resistance of plasma-treated collagen under a sodium hypochlorite (NaClO) challenge. We assessed the beneficial effect of NTAPP treatment on the acid-etched dentin–bonding interface by testing the micro-tensile bond strength and examining the morphology. We found that the immediate bonding strength of the dentin significantly increased after NTAPP treatment. Compared with the control group, NTAPP resulted in a more prominent effect on the bonding durability of the dentin–adhesive interface after treatment for 5 or 10 s. Simultaneously, the mechanical strength of dentin collagen under the NaClO challenge was improved. Our results indicate that, in optimal conditions, NTAPP could be a promising method to protect dentin collagen and to improve the bonding durability between dentin and etch-and-rinse adhesives.     

Simulation of the effects of different substrates,temperature,and substrate roughness on the mechanical properties of Al_2O_3 coating as tritium penetration barrier

Residual thermal stress in the system is a serious problem that affects the application of tritium permeation barrier coatings in fusion reactors. The stress not only determines the adhesion between coating and substrate, but also changes the properties of the material. In this study,finite element analysis was used to investigate the relationship between the residual thermal stress and the mechanical properties of Al_2O_3 tritium penetration barrier systems. Moreover, the residual thermal stress influenced by factors such as different substrates, temperature, and substrate roughness was also analyzed. The calculation showed that the hardness and elastic modulus increased with increasing compressive stress. However, the hardness and elastic modulus decreased with increasing tensile stress. The systems composed of Al_2O_3 coatings and different substrates exhibited different trends in mechanical properties. As the temperature increased, the hardness and the elastic modulus increased in an Al_2O_3/316 L stainless steel system; the trend was opposite in an Al_2O_3/Si system.Apart from this, the roughness of the substrate surface in the system could magnify the change in hardness and elastic modulus of the coating. Results showed that all these factors led to variation in the mechanical properties of Al_2O_3 tritium permeation barrier systems. Thus, thedetailed reasons for the changes in mechanical properties of these materials need to be analyzed.     

Potential of direct metal deposition technology for manufacturing thick functionally graded coatings and parts for reactors components

Direct metal deposition (DMD) is an automated 3D deposition process arising from laser cladding technology with co-axial powder injection to refine or refurbish parts. Recently DMD has been extended to manufacture large-size near-net-shape components. When applied for manufacturing new parts (or their refinement), DMD can provide tailored thermal properties, high corrosion resistance, tailored tribology, multifunctional performance and cost savings due to smart material combinations. In repair (refurbishment) operations, DMD can be applied for parts with a wide variety of geometries and sizes. In contrast to the current tool repair techniques such as tungsten inert gas (TIG), metal inert gas (MIG) and plasma welding, laser cladding technology by DMD offers a well-controlled heat-treated zone due to the high energy density of the laser beam. In addition, this technology may be used for preventative maintenance and design changes/up-grading. One of the advantages of DMD is the possibility to build functionally graded coatings (from 1 mm thickness and higher) and 3D multi-material objects (for example, 100 mm-sized monolithic rectangular) in a single-step manufacturing cycle by using up to 4-channel powder feeder. Approved materials are: Fe (including stainless steel), Ni and Co alloys, (Cu,Ni 10%), WC compounds, TiC compounds. The developed coatings/parts are characterized by low porosity (<1%), fine microstructure, and their microhardness is close to the benchmark value of wrought alloys after thermal treatment (Co-based alloy Stellite, Inox 316L, stainless steel 17-4PH). The intended applications concern cooling elements with complex geometry, friction joints under high temperature and load, light-weight mechanical support structures, hermetic joints, tubes with complex geometry, and tailored inside and outside surface properties, etc.     

Fabrication of SiC–SiC composites for fuel cladding in advanced reactor designs

Both advanced fission reactor concepts and fusion energy systems demand materials that can survive extremely harsh operating environments having persistent high temperature and high neutron flux conditions. Silicon carbide fiber/silicon carbide matrix (SiC–SiC) composites have shown promise for these applications, which include fuel cladding and reactor structural components. However, the composite fabrication process is time consuming and the fabrication of complicated geometries can be difficult.In this work, SiC–SiC and carbon fiber–SiC composite samples were fabricated using chemical vapor infiltration (CVI), and the mechanical and thermal properties of samples with a range of densities and total infiltration times were characterized and compared. Both sample density and the reinforcing fiber material were found to have a very significant influence on the composite mechanical and thermal material properties. In particular, internal porosity is found to have a significant effect on the mechanical response, as can be observed in the crack propagation in low density samples. In order to better understand the densification of the composites, a computer model is being developed to simulate the diffusion of reactants through the fiber preform, and SiC deposition on the fiber surfaces. Preliminary modeling has been correlated with experimental results and shows promising results.     

Thermal fatigue strength of type 304 stainless steel in simulated BWR environment

Thin-walled cylindrical carbon steel specimens were thermally fatigued in a pressurized autoclave. Since high and low temperature pure water were alternately supplied into the autoclave, the specimens were subjected to homogeneous thermal stress through the wall thickness. The thermal fatigue life was defined as the number of cycles to crack penetration to the inside of the cylindrical specimen. The thermal fatigue strength was compared with the mechanical fatigue strength performed in air and in high temperature water. Even if taking account of the Higuchi-Iida formula, which considers the effects of strain rate, dissolved oxygen concentration and water temperature on fatigue life, the thermal fatigue lives of carbon steel were found to be slightly shorter than the mechanical fatigue lives.     

N_2O Decomposed by Discharge Plasma with Catalysts

A great deal of attention has been focused on discharge plasma as it can rapidly decompose N_2O without additives,which is not only a kind of greenhouse gas but also a kind of damages to the ozone layer.The thermal equilibrium plasma is chosen to combine with catalysts to decompose N_2O,and its characteristics are analyzed in the present paper.The results indicate that NO and NO_2 were formed besides N_2 and O_2 during N_2O decomposition when N_2O was treated merely by discharge plasma.Concentration of NO declined greatly when the discharge plasma was combined with catalysts.Results of Raman spectra analysis on CeO_2,Ce_(0.75)Zr_(0.25)O_2and Ce_(0.5)Zr_(0.5)O_2 imply that the products selectivity has been obviously improved in discharge plasma decomposing N_2O because of the existence of massive oxygen vacancies over the composite oxide catalysts.     

Mechanical Analysis for ITER Lower CC Feeder

ITER correction coils (CCs) feeder is the important component of ITER feeder systems to supply the cryogens and electrical power for CCs. They should withstand the huge electromagnetic (EM) force and high thermal shrinkage. Considering the EM and thermal loads, mechanical analysis is performed to qualify the structural strength of the lower CC feeder. Results show that containment duct and cryopipe can meet the static criteria but busbar jacket cannot meet. It is proposed that more supports should be added at the corners for the busbar. Basically, the lower CC feeder design is valid and feasible.