The influence of moisture on atmospheric pressure plasma etching of PA6 films

The moisture in the substrate material may have a potential influence on atmospheric pressure plasma treatment. In order to investigate how the existence of moisture affects atmospheric pressure plasma treatment, polyamide 6 (PA6) films were treated by helium, helium/oxygen (O₂) plasmas using atmospheric pressure plasma jet (APPJ) at different moisture regain. The film surfaces were investigated using contact-angle measurements, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) to characterize the surfaces. The exposure of PA6 film surfaces to the plasmas led to the etching process on the surfaces and changes in the topography of the surfaces. It was shown that the etching rate and the surface roughness were higher for the 9.33% moisture regain (relative humidity 100%) group than that of the 1.61% moisture regain (relative humidity 10%) group with the same plasma gas and power.     

Surface modification of a polyamide 6 film by He/CF4 plasma using atmospheric pressure plasma jet

Polyamide 6 (PA 6) films are treated with helium(He)/CF₄ plasma at atmospheric pressure. The samples are treated at different treatment times. The surface modification of the PA 6 films is evaluated by water contact angle, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The etching rate is used to study the etching effect of He/CF₄ plasma on the PA 6 films. The T-peel strengths of the control and plasma treated films are measured to show the surface adhesion properties of the films. As the treatment time increases, the etching rate decreases steadily, the contact angle decreases initially and then increases, while the T-peel strength increases first and then decreases. AFM analyses show that the surface roughness increases after the plasma treatment. XPS analyses reveal substantial incorporation of fluorine and/or oxygen atoms to the polymer chains on the film surfaces.     

Influence of aramid fiber moisture regain during atmospheric plasma treatment on aging of treatment effects on surface wettability and bonding strength to epoxy

One of the main differences between a low-pressure plasma treatment and an atmospheric pressure plasma treatment is that in atmosphere, the substrate material may absorb significant amount of water which may potentially influence the plasma treatment effects. This paper investigates how the moisture absorbed by aramid fibers during the atmospheric pressure plasma treatment influences the aging behavior of the modified surfaces. Kevlar 49 fibers with different moisture regains (MR) (0.5, 3.5 and 5.5%, respectively) are treated with atmospheric pressure plasma jet (APPJ) with helium as the carrier gas and oxygen as the treatment gas. Surface wettability and chemical compositions, and interfacial shear strengths (IFSS) to epoxy for the aramid fibers in all groups are determined using water contact angle measurements, X-ray photoelectron spectroscopy (XPS), and micro-bond pull out tests, respectively. Immediately after the plasma treatment, the treated fibers have substantially lower water contact angles, higher surface oxygen and nitrogen contents, and larger IFSS to epoxy than those of the control group. At the end of 30 day aging period, the fibers treated with 5.5% moisture regain had a lower water contact angle and more polar groups on the fiber surface, leading to 75% improvement of IFSS over the control fibers, while those for the 0.5 and 3.5% moisture regain groups were only 30%.     

Influence of jet-to-substrate distance on plasma etching of polyamide 6 films with atmospheric pressure plasma

In this study, polyamide 6 films were treated with different jet-to-substrate distances to investigate how it influenced the etching effect of plasma treatment. When the samples were too close or too far from the nozzle, the etching rate was almost not measurable. When the distance was 2 mm, the etching rate was larger than that of other distance. Decrease in contact angle was observed under 2 mm or 3 mm of jet-to-substrate distance. However, the contact angle had no change when jet-to-substrate distance was 1 mm or 6 mm. It can be seen that the peel strength increased when jet-to-substrate distance was 2 mm or 3 mm, and the peel strength was the largest when jet-to-substrate distance was 2 mm. However, the peel strength had no change when jet-to-substrate distance was 1 mm or 6 mm. These results were corresponding to SEM and XPS results.     

电子回旋共振微波等离子体刻蚀α:CH薄膜的工艺

为了刻蚀出图形完整、侧壁陡直、失真度小的α:CH薄膜微器件,研究了有铝和无铝掩膜、气体流量比、工作气压对刻蚀速率的影响,并对纯氧等离子体刻蚀稳定性进行了研究。研究结果表明：在相同条件下,刻蚀速率随刻蚀时间变化不大;a:CH薄膜上有铝和无铝掩膜时,刻蚀速率相同;流量一定时,刻蚀速率随氩气和氧气体积比的增大而降低,当用纯氩气时,几乎没刻蚀作用;刻蚀速率随工作气压的增大而降低。实验中,得到最佳刻蚀条件是：纯氧气,流量4 mL·s-1,工作气压9.9×10-2 Pa,微波源电流80 mA,偏压-90 V。     

Modification of surface properties of polyamide 6 films with atmospheric pressure plasma

To investigate the effect of the different plasma gases treatment on the surface modification of atmospheric pressure plasma, polyamide 6 films were treated using pure helium (He), He/O₂ and He/CF₄, respectively. Atomic force microscopy (AFM) showed rougher surface, while X-ray photoelectron spectroscopy (XPS) revealed increased oxygen and fluorine contents after the plasma treatments. The plasma treated samples had lower water contact angles and higher T-peel strength than that of the control. The addition of small amount of O₂ or CF₄ to He plasma increases the effectiveness of the plasma treatment in polymer surface modification in terms of surface roughness, surface hydrophilic groups, etching rate, water contact angle and bonding strength.     

Effect of H2 and O2 plasma etching treatment on the surface of diamond-like carbon thin film

In this study, we investigated the surface properties of diamond-like carbon (DLC) films for biomedical applications through plasma etching treatment using oxygen (O₂) and hydrogen (H₂) gas. The synthesis and post-plasma etching treatment of DLC films were carried out by 13.56 MHz RF plasma enhanced chemical vapor deposition (PECVD) system. In order to characterize the surface of DLC films, they were etched to a thickness of approximately 100 nm and were compared with an as-deposited DLC film. We obtained the optimum condition through power variation, at which the etching rate by H₂ and O₂ was 30 and 80 nm/min, respectively. The structural and chemical properties of these thin films after the plasma etching treatment were evaluated by Raman and Fourier transform infrared (FT-IR) spectroscopy. In the case of as-deposited and H₂ plasma etching-treated DLC film, the contact angle was 86.4° and 83.7°, respectively, whereas it was reduced to 35.5° in the etching-treated DLC film in O₂ plasma. The surface roughness of plasma etching-treated DLC with H₂ or O₂ was maintained smooth at 0.1 nm. These results indicated that the surface of the etching-treated DLC film in O₂ plasma was hydrophilic as well as smooth.     

Diagnostics of Low-Pressure Oxygen RF Plasmas and the Mechanism for Polymer Etching: A Comparison of Reactive Sputter Etching and Magnetron Sputter Etching

We have compared low-pressure oxygen RF plasmas and the etching of photoresist in a reactive sputter etch reactor and in a magnetron etch reactor using Langmuir probe, optical emission actinometry, and mass spectrometry measurements. The Langmuir probe data allow the determination of the plasma ion density and electron temperature, and thus the ion flux onto the substrate. The optical data yield information on the presence of O atoms and O2+ ions. Stable reactant and product species are monitored with a mass spectrometer. The main difference between the two reactors is that in magnetron sputter etching (MSE), the ion flux to the substrate is about an order of magnitude higher, under comparable plasma conditions, than in reactive sputter etching (RSE). This accounts for the higher etch rate in MSE. However, the etch yield per ion is higher in RSE because of the higher ion energy. Etch rates correlate neither with the ion flux to the substrate nor with the density of O atoms in the plasma, but change in parallel with the consumption of reactant gas. We conclude that in etching a polymer in a low-pressure oxygen plasma, the main neutral reactant species are O2 molecules, and an important role of the ions is to remove reaction products from the substrate surface.     

Elucidating surface properties of dry-etched ZnO using H2/CH4 and H2/CH4/Ar plasma

This paper reports a study of reactive ion etching (RIE) of n-ZnO in H₂/CH₄ and H₂/CH₄/Ar gas mixtures. Variables in the experiment were gas flow ratios, radio-frequency (rf) plasma power, and total pressure. Structural and electrical parameters of the etched surfaces and films were determined. Both the highest surface roughness and highest etching rate of ZnO films were obtained with a maximum rf power of 300 W, but at different gas flow ratios and working pressures. These results were expected because increasing the rf power increased the bond-breaking efficiency of ZnO. The highest degree of surface roughness was a result of pure physical etching by H₂ gas without mixed CH₄ gas. The highest etching rate was obtained from physical etching of H₂/Ar species associated with chemical reaction of CH₄ species. Additionally, the H₂/CH₄/Ar plasma treatment drastically decreased the specific contact and sheet resistance of the ZnO films. These results indicated that etching the ZnO film had roughened the surface and reduced its resistivity to ohmic contact, supporting the application of a roughened transparent contact layer (TCL) in light-emitting diodes (LEDs).     

Modification of surface properties of polypropylene (PP) film using DC glow discharge air plasma

The industrial use of polypropylene (PP) films is limited because of undesirable properties such as poor adhesion and printability. In the present study, a DC glow discharge plasma has been used to improve the surface properties of PP films and make it useful for technical applications. The change in hydrophilicity of modified PP film surface was investigated by contact angle (CA) and surface energy measurements as a function of exposure time. In addition, plasma-treated PP films have been subjected to an ageing process to determine the durability of the plasma treatment. Changes in morphological and chemical composition of PP films were analyzed by atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The improvement in adhesion was studied by measuring T-peel and lap shear strength. The results show that the surface hydrophilicity has been improved due to the increase in the roughness and the introduction of oxygen-containing polar groups. The AFM observation on PP film shows that the roughness of the surface increased due to plasma treatment. Analysis of chemical binding states and surface chemical composition by XPS showed an increase in the formation of polar functional groups and the concentration of oxygen content on the plasma-processed PP film surfaces. T-peel and lap shear test for adhesion strength measurement showed that the adhesion strength of the plasma-modified PP films increased compared with untreated films surface.     

刻蚀AlN缓冲层对硅衬底N极性n-GaN表面粗化的影响

研究了等离子体刻蚀AlN缓冲层对硅衬底N极性n-GaN表面粗化行为的影响. 实验结果表明, 表面AlN缓冲层的状态对N极性n-GaN的粗化行为影响很大, 采用等离子体刻蚀去除一部分表面AlN缓冲层即可以有效提高N极性n-GaN在KOH溶液中的粗化效果, AlN缓冲层未经任何刻蚀处理的样品粗化速度过慢, 被刻蚀完全去除AlN缓冲层的样品容易出现粗化过头的现象. 经X射线光电子能谱分析可知, 等离子体刻蚀能够提高样品表面AlN缓冲层Al 2p的电子结合能, 使得样品表面费米能级向导带底靠近, 原子含量测试表明样品表面产生了大量的N空位, N空位提供电子, 使得材料表面费米能级升高, 这降低了KOH溶液和样品表面之间的肖特基势垒, 从而有利于表面粗化的进行. 通过等离子体刻蚀掉表面部分AlN缓冲层, 改善了N极性n-GaN在KOH溶液中的粗化效果, 明显提升了对应发光二级管器件的出光功率.     

Surface properties of platinum thin films as a function of plasma treatment conditions

We examined the surface properties of platinum (Pt) thin films exposed to oxygen and argon plasma treatments and compared them to as-deposited Pt films. The surface wetting properties, refractive index and extinction coefficient of the Pt films were monitored as a function of time after different plasma treatments. Surfaces treated with an oxygen plasma were dramatically different from as-deposited Pt, whereas argon plasma treated surfaces were similar to as-deposited films. X-ray photoelectron spectroscopy confirmed the formation of platinum oxide on films treated with an oxygen plasma, while such oxide diminished after argon plasma treatment. Surface morphology studied with atomic force microscopy indicated a strong dependence of the surface roughness of the Pt films on the power and duration of the argon plasma used for the treatment. Based on these studies, an oxygen plasma treatment followed by a brief low-power argon plasma etch was developed for the purpose of regenerating clean and metallic Pt surfaces, and at the same time providing the smoothest possible surface morphology.     

Influence of hydrogenation on the structure and visible photoluminescence of germanium oxide thin films

Substoichiometric germanium oxide thin films were prepared by evaporation of GeO₂ powder. The as-deposited samples showed a luminescence band in the visible range. Hydrogen was used to passivate the dangling bond defects and therefore to determine the origin of photoluminescence in the germanium oxide films. Hydrogen was introduced in the films from an electron cyclotron resonance (ECR) plasma source during or after the evaporation. The films hydrogenated during evaporation contain little oxygen because of an etching mechanism. In the post-hydrogenated films, the oxygen content is higher. With the hydrogenation treatment, the oxygen dangling bonds are suppressed. It is proposed that the photoluminescence in the visible range is attributed to the structural defects.     

Low power gas discharge plasma mediated inactivation and removal of biofilms formed on biomaterials

The antibacterial activity of gas discharge plasma has been studied for quiet some time. However, high biofilm inactivation activity of plasma was only recently reported. Studies indicate that the etching effect associated with plasmas generated represent an undesired effect, which may cause live bacteria relocation and thus contamination spreading. Meanwhile, the strong etching effects from these high power plasmas may also alter the surface chemistry and affect the biocompatibility of biomaterials. In this study, we examined the efficiency and effectiveness of low power gas discharge plasma for biofilm inactivation and removal. Among the three tested gases, oxygen, nitrogen, and argon, discharge oxygen demonstrated the best anti-biofilm activity because of its excellent ability in killing bacteria in biofilms and mild etching effects. Low power discharge oxygen completely killed and then removed the dead bacteria from attached surface but had negligible effects on the biocompatibility of materials. DNA left on the regenerated surface after removal of biofilms did not have any negative impact on tissue cell growth. On the contrary, dramatically increased growth was found for these cells seeded on regenerated surfaces. These results demonstrate the potential applications of low power discharge oxygen in biofilm treatments of biomaterials and indwelling device decontaminations.     

Two-dimensional simulation of polysilicon etching with chlorine ina high density plasma reactor

A two-dimensional fluid simulation of polysilicon etching with chlorine in an inductively-coupled high density plasma source is presented. A modular approach was used to couple in a self-consistent manner the disparate time scales of plasma and neutral species transport. This way, complex plasma chemical reactions (involving electrons, ions and neutrals) as well as surface chemistry can be included in the simulation, The power deposited into the plasma was calculated by an electromagnetics module which solves Maxwell's equations. The power deposition was used in the electron energy module to find the electron temperature and the rate coefficients of electron-impact reactions. These were in turn used as source terms in separate neutral and charged species transport modules. By iterating among the modules, a self-consistent solution was obtained. Quantities of interest, such as power deposition, species density and flux, and etch rate and uniformity were thus calculated, As power deposition was increased, the electron density increased linearly, the plasma became less electronegative, the degree of gas dissociation increased, and the plasma potential remained constant. The radial uniformity of the Cl atom flux was better than that of the ion flux. The reactivity of the wafer as compared to that of the surrounding electrode surface significantly affected the etch uniformity, despite the low pressure of 10 mtorr     

Effect of argon ion activity on the properties of Y2O3 thin films deposited by low pressure PACVD

Yttrium oxide thin films are deposited by microwave electron cyclotron resonance (ECR) plasma assisted metal organic chemical vapour deposition process using an indegeneously developed Y(thd)₃ {(2,2,6,6-tetramethyl-3,5-heptanedionate)yttrium} precursor. Depositions were carried out at two different argon gas flow rates keeping precursor and oxygen gas flow rate constant. The deposited coatings are characterized by X-ray photoelectron spectroscopy (XPS), glancing angle X-ray diffraction (GIXRD) and infrared spectroscopy. Optical properties of the films are studied by spectroscopic ellipsometry. Hardness and elastic modulus of the films are measured by load depth sensing nanoindentation technique. Stability of the film and its adhesion with the substrate is inferred from the nanoscratch test.It is shown here that, the change in the argon gas flow rates changes the ionization of the gas in the microwave ECR plasma and imposes a drastic change in the characteristics like composition, structure as well as mechanical properties of the deposited film.     

氧等离子体处理对GaAs表面单层自组装SiO2纳米球薄膜的影响

二维纳米阵列结构因其重要的光学性能被广泛应用于各类光电子器件。本文对自组装单层SiO2纳米球掩模刻蚀法制备GaAs纳米柱二维阵列结构的关键工艺技术进行了研究。采用旋涂法在GaAs表面制备自组装单层SiO2纳米球,重点研究了GaAs表面氧等离子体亲水处理工艺对纳米球排列特性的影响,获得最佳工艺条件为功率配比100 W+80 W、腔室压力4 Pa、氧气流量20 mL/min、处理时间1200 s,并最终得到排列紧密的大面积单层纳米球薄膜。以单层纳米球为掩模,采用感应耦合等离子体刻蚀技术在GaAs表面制备了纳米柱阵列并测试了其表面光反射谱。测试结果表明,GaAs纳米柱阵列在特定波段的反射率降低至5%,远低于表面无纳米结构的薄膜材料表面高达40%的光反射。分析表明纳米柱可以激发米氏散射共振效应,从而有效降低反射率并提升光吸收。     

Effect of process parameters on surface morphology and characterization of PE-ALD SnO2 thin films for gas sensing

Tin dioxide (SnO₂) thin films were deposited by plasma enhanced-atomic layer deposition (PE-ALD) on Si(1 0 0) substrate using dibutyl tin diacetate (DBTA) ((CH₃CO₂)₂Sn[(CH₂)₃-CH₃]₂) as precursor. The process parameters were optimized as a function of substrate temperature, source temperature and purging time. It is observed that the surface phenomenon of the thin films was changed with film thickness. Atomic force microscopy (AFM) images and X-ray diffraction (XRD) pattern were used to observe the texture and crystallanity of the films. The films deposited for 100, 200 and 400 cycles were characterized by XPS to determine the chemical bonding properties. XPS results reveal that the surface dominant oxygen species for 100, 200 and 400 cycles deposited films are O₂⁻, O⁻ and O²⁻, respectively. The 200 cycles film has exhibited highest concentration of oxygen (O⁻) species before and after annealing. Conductivity studies revel that this film has best adsorption strength to the oxygen ions forming on the surface. The sensor with 200 cycles SnO₂ thin film has shown highest sensitivity to CO gas than other films. A correlation between the characteristics of Sn3d_5/2 and O1s XPS spectra before and after annealing and the electrical behavior of the SnO₂ thin films is established.     

Atmospheric air-plasma treatment of polyester fiber to improve the performance of nanoemulsion silicone

Influence of atmospheric air plasma treatment on performance of nanoemulsion silicone softener on polyethylene terephthalate fibers was investigated by the use of fourier transform infrared spectroscopy (FTIR), bending lengths (BL), wrinkle recovery angles (WRA), fiber friction coefficient analysis (FFCA), moisture absorbency (MA), scanning electron microscopy (SEM) and reflectance spectroscopy (RS). Results indicated that the plasma pretreatment modifies the surface of fibers and increases the reactivity of substrate toward nanoemulsion silicone. Moisture regain and microscopic tests showed that the combination of plasma and silicone treatments on polyethylene terephthalate can decrease moisture absorption due to uniform coating of silicone emulsion on surface of fibers.     

A comparative study of the physical properties of Sb2S3 thin films treated with N2 AC plasma and thermal annealing in N2

As-deposited antimony sulfide thin films prepared by chemical bath deposition were treated with nitrogen AC plasma and thermal annealing in nitrogen atmosphere. The as-deposited, plasma treated, and thermally annealed antimony sulfide thin films have been characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy, scanning electron microscopy, atomic force microscopy, UV-vis spectroscopy, and electrical measurements. The results have shown that post-deposition treatments modify the crystalline structure, the morphology, and the optoelectronic properties of Sb₂S₃ thin films. X-ray diffraction studies showed that the crystallinity of the films was improved in both cases. Atomic force microscopy studies showed that the change in the film morphology depends on the post-deposition treatment used. Optical emission spectroscopy (OES) analysis revealed the plasma etching on the surface of the film, this fact was corroborated by the energy dispersive X-ray spectroscopy analysis. The optical band gap of the films (E_g) decreased after post-deposition treatments (from 2.36 to 1.75 eV) due to the improvement in the grain sizes. The electrical resistivity of the Sb₂S₃ thin films decreased from 10⁸ to 10⁶ Ω-cm after plasma treatments.