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Fluorine-free superhydrophobic surfaces by atmospheric pressure plasma deposition of silazane-based suspensions 通过常压等离子体沉积硅烷基悬浮液实现无氟超疏水性表面
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-27 DOI: 10.1016/j.apsadv.2024.100645
Camilo Rendon Piedrahita, Kamal Baba, Robert Quintana, Patrick Choquet
Atmospheric plasma is used to deposit superhydrophobic fluorine-free thin films onto a substrate. In this process, a suspension of micron size silica particles in a silazane based precursor is deposited in a single step using a dielectric barrier discharge plasma jet moving above the substrate. Thanks to an optimized configuration between the suspension injection and the plasma jet, the silazane precursor can be polymerized on the substrate surface but also, on silica particles to form additional micro size particles. The experimental parameters for optimal deposition are discussed, with emphasis on those leading to the formation of this dual roughness surface caused by the arrangement of both silica particles and particles generated from the precursor plasma polymerization. The combination of these two different length scales for the roughness leads to a decreased wettability of the coated substrate and a water contact angle larger than 150°.
大气等离子体用于在基底上沉积超疏水无氟薄膜。在这一工艺中,使用在基底上方移动的介质阻挡放电等离子体射流,将微米大小的二氧化硅颗粒悬浮在硅氮烷前体中,一步完成沉积。由于优化了悬浮液喷射和等离子体喷射之间的配置,硅烷前驱体不仅能在基底表面聚合,还能在二氧化硅颗粒上形成额外的微小颗粒。本文讨论了优化沉积的实验参数,重点是硅颗粒和前驱体等离子聚合产生的颗粒的排列所导致的双重粗糙表面的形成。这两种不同长度尺度的粗糙度结合在一起,导致涂层基底的润湿性降低,水接触角大于 150°。
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引用次数: 0
Current-voltage plots reveal details of the energy level alignment during photoelectron spectroscopy experiments 电流电压图揭示光电子能谱实验中能级排列的细节
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-24 DOI: 10.1016/j.apsadv.2024.100643
Grzegorz Greczynski
The photoelectron current Is emitted from samples exposed to soft X-rays, such as is the case during X-ray photoelectron spectroscopy (XPS) analyses, is dominated by secondary electrons (SE) with energies not exceeding several eVs. Because of that, both the magnitude and the direction of Is is highly sensitive to the applied sample bias Vs with the magnitude of just a few volts. By measuring current-voltage characteristics for a series of samples with different work functions ϕSA a clear correlation between ϕSA and the shape of the IsVs curves is demonstrated. While all IsVs plots have a characteristic “reversed S” shape, a clear and consistent shift towards positive Vs values is observed with increasing ϕSA. The effect is explained by variations in the contact potential Vc established between the sample and the spectrometer. For all samples there is an excellent agreement between the Vc values (derived by ultraviolet photoelectron spectroscopy from the SE cut-offs) and the critical Vs value at which the photocurrent begins to drop. Hence, simple to perform current-voltage measurements, provide a unique insight into the details of the energy level alignment between sample and the spectrometer. In particular, the sign and the magnitude of the contact potential as well as relative changes in the sample work function can be determined. The knowledge of these parameters is often essential for correct interpretation of XPS spectra.
暴露在软 X 射线下的样品(例如在 X 射线光电子能谱(XPS)分析过程中)发出的光电子电流 Is 主要由能量不超过几 eV 的次级电子(SE)构成。因此,Is 的大小和方向对施加的样品偏压 Vs 非常敏感,其大小仅为几伏。通过测量一系列具有不同工作函数 ϕSA 的样品的电流-电压特性,可以清楚地看出 ϕSA 与 Is-Vs 曲线形状之间的相关性。虽然所有的 Is-Vs 曲线图都具有 "反向 S "形状的特征,但随着 ϕSA 的增大,Vs 值明显一致地向正值偏移。样品和光谱仪之间建立的接触电势 Vc 的变化可以解释这种效应。对于所有样品,Vc 值(通过紫外光电子能谱从 SE 截断点得出)与光电流开始下降的临界 Vs 值之间非常一致。因此,通过简单的电流-电压测量,可以深入了解样品与光谱仪之间能级排列的细节。尤其是可以确定接触电势的符号和大小,以及样品功函数的相对变化。了解这些参数往往对正确解读 XPS 光谱至关重要。
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引用次数: 0
Investigation of mechanical morphological structural and electrochemical properties of PVD TiAlN coating: A detail experimental and its correlation with an analytical approach using the least square method 研究 PVD TiAlN 涂层的机械形态结构和电化学性能:详细实验及其与使用最小二乘法的分析方法的相关性
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-20 DOI: 10.1016/j.apsadv.2024.100638
Soham Das , Soumya Kanti Biswas , Abhishek Kundu , Ranjan Ghadai , Spandan Guha

In this experimental investigation, a Physical Vapor Deposition (PVD) process was employed to deposit TiAlN coating onto a Si substrate. The nitrogen flow rate, bias voltage, and substrate-to-target distance were selected as input parameters, each with three different levels. The design of these input parameters was structured according to Taguchi's L9 Orthogonal Array (OA). Following deposition, the mechanical, microstructural, structural, and electrochemical properties of the TiAlN coating were meticulously characterized and analyzed to discern the influence of the selected parameters on its various properties. Microstructural analysis revealed a homogeneous structure throughout the film. Additionally, the mechanical properties of the film exhibited notable performance under the specified parameters. However, it was observed that no consistent trend could be identified across different properties concerning the applied parameters. To elucidate the complex relationships among these variables, the Least Squares Method (LSM) regression analysis technique was employed. This analytical approach facilitated the establishment of correlations among the diverse parameters, enhancing the understanding of their collective impact on the TiAlN coating properties. The understanding of analytical results will be useful for predicting the values between the two extremities to measure the performance parameters where the experimental results are not available.

在这项实验研究中,采用了物理气相沉积(PVD)工艺在硅基底上沉积 TiAlN 涂层。氮气流速、偏置电压和基底到目标的距离被选为输入参数,每个参数有三个不同的水平。这些输入参数的设计采用田口 L9 正交阵列(OA)结构。沉积后,对 TiAlN 涂层的机械、微观结构、结构和电化学特性进行了细致的表征和分析,以确定所选参数对其各种特性的影响。微观结构分析表明,整个薄膜具有均匀的结构。此外,在特定参数下,薄膜的机械性能也表现出显著的性能。然而,观察发现,在应用参数的不同特性之间并没有发现一致的趋势。为了阐明这些变量之间的复杂关系,我们采用了最小二乘法(LSM)回归分析技术。这种分析方法有助于建立不同参数之间的相关性,从而加深理解这些参数对 TiAlN 涂层性能的共同影响。对分析结果的理解将有助于预测两个极值之间的数值,从而在没有实验结果的情况下测量性能参数。
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引用次数: 0
As-deposited and dewetted Cu layers on plasma treated glass: Adhesion study and its effect on biological response 等离子处理玻璃上的砷沉积和脱水铜层:附着力研究及其对生物反应的影响
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-18 DOI: 10.1016/j.apsadv.2024.100639
Alena Reznickova , Veronika Lacmanova , Marie Hubalek Kalbacova , Petr Hausild , Jiri Nohava , Zdenka Kolska , Anna Kutova , Petr Slepicka

Improving the adhesion of nanosized copper films to a glass substrate is vital for their application in electronics and medicine, as it enhances their overall reliability. For this purpose, we employed Ar plasma etching (240 s) and magnetron sputtering to create copper layers on a glass substrate. Furthermore, we investigated the effect of subsequent solid state dewetting (at 300 °C) of Cu nanolayers on the interface stability. Increasing the sputtering time resulted in elevated copper concentration, UV-Vis absorption, conductivity, and surface roughness. The as-deposited and dewetted samples exhibited very good wettability with water contact angles below 60°. Importantly, plasma treatment improved the adhesion of the Cu layers to the glass. Subsequent dewetting accelerated surface diffusion and the oxidation of Cu atoms, causing structural and morphological changes. The presence of CuO after dewetting caused loss of the surface plasmon resonance (SPR) band in the UV-Vis spectrum and a decrease in sample conductivity due to the transformation of the copper layer from a metal to an oxide. Biological testing revealed a more pronounced bactericidal effect for the as-deposited Cu layer against E. coli and S. epidermidis on contrary to dewetted samples. The similar cytotoxic trend was observed for human dermal fibroblasts and hepatocytes. Nonetheless, biological testing confirmed better cell adhesion on dewetted Cu layers compared to the as-deposited ones. Therefore, our copper nanostructured samples could find application as antibacterial coatings of biomedical devices.

提高纳米铜膜与玻璃基底的附着力对其在电子和医药领域的应用至关重要,因为这可以增强其整体可靠性。为此,我们采用了氩等离子刻蚀(240 秒)和磁控溅射技术在玻璃基底上形成铜层。此外,我们还研究了铜纳米层后续固态脱胶(300 °C)对界面稳定性的影响。增加溅射时间会导致铜浓度、紫外可见吸收率、电导率和表面粗糙度升高。经过沉积和脱水处理的样品具有非常好的润湿性,水接触角低于 60°。重要的是,等离子处理提高了铜层与玻璃的附着力。随后的脱水加速了铜原子的表面扩散和氧化,导致结构和形态发生变化。脱水后 CuO 的存在导致紫外-可见光谱中表面等离子体共振 (SPR) 波段的消失,同时由于铜层从金属转变为氧化物,样品的导电性降低。生物测试表明,与经过脱水处理的样品相比,经过沉积的铜层对大肠杆菌和表皮葡萄球菌具有更明显的杀菌效果。人类真皮成纤维细胞和肝细胞也观察到了类似的细胞毒性趋势。不过,生物测试证实,与沉积后的铜层相比,脱水后的铜层具有更好的细胞粘附性。因此,我们的纳米铜结构样品可用作生物医学设备的抗菌涂层。
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引用次数: 0
Concomitant silanization and controlled fibronectin adsorption on S53P4 bioactive glass enhances human adipose stem cells spreading and differentiation 在 S53P4 生物活性玻璃上同时进行硅烷化和可控纤连蛋白吸附可促进人类脂肪干细胞的扩散和分化
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-01 DOI: 10.1016/j.apsadv.2024.100635
Virginia Alessandra Gobbo , Amel Houaoui , Kimiya Tajik , Vesa P. Hytönen , Susanna Miettinen , Jonathan Massera

Orthopedic disorders are increasing in our society due to population aging. Numerous biomaterials have been developed to support bone regeneration, however showing a strong discrepancy between in vitro and in vivo results. This has been attributed to a lack of knowledge about protein adsorption, an early step occurring after biomaterial implantation. Bioactive glass S53P4 is clinically accepted for orthopedic applications pertaining to its osteoconductive and osteogenic behavior. However, its interactions with proteins are still unclear. To better understand the impact of surface chemistry on the glass-protein interactions, bare and silanized S53P4 were placed in contact with fibronectin (fn), in static and dynamic conditions. The surfaces were characterized by zeta potential, confocal microscopy and FTIR-ATR spectroscopy.The impact of fn on the cell response was assessed by live-dead, proliferation and morphology tests, using human adipose stem cells (hASCs). Both S53P4 and silanized-S53P4 showed good cell viability. Fn was found to affect cell alignment on both bare and silanized substrates. The impact of the surface treatments on osteogenesis was evaluated studying the expression of relevant osteogenic markers (hDLX5, hRUNX2A, hOSTERIX), which was particularly promoted by the concomitant action of silanization and fn coating.

由于人口老龄化,骨科疾病在我们的社会中日益增多。目前已开发出许多支持骨再生的生物材料,但体外结果与体内结果之间存在很大差异。这归因于人们对蛋白质吸附缺乏了解,而蛋白质吸附是生物材料植入后的早期阶段。生物活性玻璃 S53P4 具有骨诱导性和成骨性,已被临床应用于骨科领域。然而,它与蛋白质的相互作用仍不清楚。为了更好地了解表面化学对玻璃与蛋白质相互作用的影响,我们在静态和动态条件下将裸露和硅烷化的 S53P4 与纤连蛋白(fn)接触。使用人脂肪干细胞(hASCs)通过活死、增殖和形态测试评估了 fn 对细胞反应的影响。S53P4和硅烷化-S53P4都显示出良好的细胞活力。研究发现,Fn 会影响裸基底和硅烷化基底上的细胞排列。通过研究相关成骨标志物(hDLX5、hRUNX2A、hOSTERIX)的表达,评估了表面处理对成骨的影响。
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引用次数: 0
TENG-driven single-droplet green electrochemical etching and deposition for chemical sensing applications 用于化学传感应用的 TENG 驱动的单液滴绿色电化学蚀刻和沉积
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-01 DOI: 10.1016/j.apsadv.2024.100634
Ruey-Chi Wang, Yi-Hong Zhou, Yu-Hsuan Lee, Hsiu-Cheng Chen, Chi-En Chen

Selected area electrochemical etching (EE) and electrochemical deposition (ED) are widely used for fabricating microstructures and devices, but they require complex processes and expensive equipment and generate significant electrolyte waste. This study demonstrates a novel single-droplet electrochemical system using a triboelectric nanogenerator (TENG) for self-powered selected area EE and ED reactions. Utilizing TENG's pulsed power, Al nanostructures were created by EE, while nano-Ag and Cu2O nanocubes were synthesized by ED. The generated nanomaterials were applied to detect trace chemicals through the Surface-Enhanced Raman Scattering effect. The electrochemical reaction area can be controlled by droplet size, and patterns can be created using a needle movement platform. The size and density of nanostructures can be adjusted by the TENG's current, collision frequency, and electrolyte concentration. The deposition gradient from the center to the edge of the droplet is controlled by the distance between the needle and the substrate. COMSOL Multiphysics calculations show that a smaller D creates a larger electric field gradient. However, the varied deposition gradients were attributed to competition of electric field, diffusion effects, and capillary flow. This proposed green technology offers low cost, simplicity, no waste electrolyte, and self-powering capabilities, pioneering new research directions in EE and ED.

选区电化学蚀刻(EE)和电化学沉积(ED)被广泛用于制造微结构和器件,但它们需要复杂的工艺和昂贵的设备,并且会产生大量电解液废物。本研究展示了一种新型单液滴电化学系统,该系统使用三电纳米发电机(TENG)为选定区域的 EE 和 ED 反应提供自供电。利用 TENG 的脉冲功率,通过 EE 生成了铝纳米结构,而通过 ED 合成了纳米银和 Cu2O 纳米立方体。生成的纳米材料通过表面增强拉曼散射效应用于检测痕量化学物质。电化学反应区域可由液滴大小控制,并可利用针移动平台创建图案。纳米结构的大小和密度可通过 TENG 的电流、碰撞频率和电解液浓度进行调节。从液滴中心到边缘的沉积梯度由针头和基底之间的距离控制。COMSOL Multiphysics 计算表明,D 越小,电场梯度越大。然而,不同的沉积梯度归因于电场竞争、扩散效应和毛细管流动。这项拟议的绿色技术具有成本低、简单、无废电解质和自供电能力等特点,开创了电子工程和教育学的新研究方向。
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引用次数: 0
Transfer of micron pattern with reactive atmospheric plasma jets into fused silica 用反应性大气等离子体射流将微米图案转移到熔融石英中
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-09-01 DOI: 10.1016/j.apsadv.2024.100636
Martin Ehrhardt , Pierre Lorenz , Joachim Zajadacz , Robert Heinke , Thomas Arnold , Klaus Zimmer

Pattern transfer by plasma etching is a traditional standard technology in microelectronics and other micron technologies. These technologies require vacuum conditions, which limit throughput, size, and low-cost fabrication. Recent developments in low cost atmospheric plasma technologies may be suitable to realize pattern transfer without vacuum conditions. Reactive atmospheric plasma jet etching has been used to transfer aluminum mask patterns to fused silica. Aluminum line patterns of 2.5 to 50 µm width on fused silica wafer are exposed to a static as well as a scanning CF4/O2 reactive atmospheric plasma jet with a footprint diameter of 0.85 mm (full width at half maximum), resulting in etching only the SiO2 and causing a nearly isotropic etch with an etch rate of about 200 nm/s. As a result, line narrowing, trapezoidal line cross-sections, and under-etching were observed. The successfully transferred line patterns with the demonstrated widths and depths are of technological interest in various fields of application. Therefore, this approach enables low-cost patterning of fused silica through the use of reactive atmospheric plasma jet etching for micron-scale pattern transfer. This advancement addresses the limitations of both traditional vacuum-based and wet etching methods.

等离子刻蚀图案转移是微电子和其他微米技术的传统标准技术。这些技术需要真空条件,从而限制了产量、尺寸和低成本制造。低成本大气等离子体技术的最新发展可能适合在无真空条件下实现图案转移。反应性大气等离子体喷射蚀刻已被用于将铝掩膜图案转移到熔融石英上。将熔融石英晶片上宽度为 2.5 至 50 微米的铝线图案暴露在静态和扫描 CF4/O2 反应性大气等离子体射流中,射流的足迹直径为 0.85 毫米(半最大全宽),结果只蚀刻了二氧化硅,并以约 200 纳米/秒的蚀刻速率产生了近乎各向同性的蚀刻。因此,观察到了线变窄、梯形线截面和蚀刻不足。成功转移的线条图案具有所展示的宽度和深度,在各个应用领域都具有技术意义。因此,这种方法通过使用反应性大气等离子体喷射蚀刻技术进行微米级图案转移,实现了熔融石英的低成本图案化。这一进步解决了传统真空蚀刻和湿蚀刻方法的局限性。
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引用次数: 0
Preface on Novel Aspects in Theoretical and Computational Surface Science (NATCSS) 理论与计算表面科学(NATCSS)新观点序言
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-08-28 DOI: 10.1016/j.apsadv.2024.100632
Seung Geol Lee , Ian Shuttleworth , Herbert M. Urbassek , Byungchan Han , Alfredo Juan
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引用次数: 0
Sand blasting for hydrophobic surface generation in polymers: Experimental and machine learning approaches 在聚合物中喷砂生成疏水表面:实验和机器学习方法
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-08-28 DOI: 10.1016/j.apsadv.2024.100633
Erencan Oranli , Chenbin Ma , Nahsan Gungoren , Asghar Heydari Astaraee , Sara Bagherifard , Mario Guagliano

Wettability is a crucial surface feature of polymers due to their numerous interaction-destined applications. This study focuses on the application of sand blasting process for investigating the wettability of polymeric materials to produce hydrophobic behavior. Four different polymeric materials, Acrylonitrile Butadiene Styrene (ABS), Poly(methyl methacrylate) (PMMA), Polypropylene (PP), and Polycarbonate (PC) underwent sand blasting with varying process parameters, following a comprehensive plan for the design of experiments. Subsequent analyses included surface roughness measurement and wettability tests, supplemented by scanning electron and confocal microscopy observations to gain deeper insights into the blasted surfaces. A predictive model based on a machine learning algorithm was developed using the backpropagation technique to correlate the surface treatment parameters to surface roughness and wettability indexes. From the experimental results sand blasting proved to be efficient in creating hydrophobic surfaces on all the tested materials. The developed neural network demonstrated high fitting degrees between the predicted and measured values. ABS exhibited the most hydrophobic behavior and emerged as a strong candidate for further investigations.

润湿性是聚合物的一个重要表面特征,因为它们有许多相互作用的用途。本研究的重点是应用喷砂工艺研究聚合物材料的润湿性,以产生疏水行为。四种不同的聚合物材料,即丙烯腈-丁二烯-苯乙烯(ABS)、聚甲基丙烯酸甲酯(PMMA)、聚丙烯(PP)和聚碳酸酯(PC),按照实验设计的综合计划,采用不同的工艺参数进行喷砂处理。随后的分析包括表面粗糙度测量和润湿性测试,并辅以扫描电子显微镜和共聚焦显微镜观察,以深入了解喷砂表面。利用反向传播技术开发了基于机器学习算法的预测模型,将表面处理参数与表面粗糙度和润湿性指标联系起来。实验结果证明,喷砂能有效地在所有测试材料上形成疏水表面。开发的神经网络在预测值和测量值之间表现出很高的拟合度。ABS 的疏水性最强,是进一步研究的有力候选材料。
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引用次数: 0
Effect of SiO2-reinforcement and alkali treatment on the corrosion resistance of plasma electrolytic oxide coating on AZ31 magnesium alloy 二氧化硅强化和碱处理对 AZ31 镁合金等离子电解氧化物涂层耐腐蚀性的影响
IF 7.5 Q1 CHEMISTRY, PHYSICAL Pub Date : 2024-08-26 DOI: 10.1016/j.apsadv.2024.100631
Sri Rahmadani, Anawati Anawati

Plasma electrolytic oxidation (PEO) produces an oxide coating containing pores and cracks lowering corrosion protection. The defects can be sealed by in-situ or post-treatment methods. This work compares the sealing effect of SiO2 particles and post-alkali treatment on the corrosion resistance of PEO coatings formed on AZ31 magnesium (Mg) alloy. PEO was conducted in a phosphate-based electrolyte containing 2 g/l nanoparticle SiO2 at a constant current density of 300 A/m2 for 10 min. The post-alkali treatment was performed in 0.5 M NaOH solution at 80 °C for 30 min. The corrosion resistance was evaluated using polarization, electrochemical impedance spectroscopy, and weight loss tests. The SiO2 particles were successfully embedded uniformly in the Mg3(PO4)2 coating, enhancing the coating compactness and stability. The reinforced coating exhibited ten times higher impedance modulus and lower corrosion current density. The post-alkali treatment improved corrosion resistance but not as high as the SiO2 reinforcement. The impedance modulus of the alkali-treated specimen increased five times, and the corrosion current density decreased three times of the base coating. The weight loss test consistently showed that the SiO2-reinforced coating generated lower mass loss during 14 days of immersion in simulated body fluid.

等离子电解氧化(PEO)产生的氧化物涂层含有气孔和裂缝,可降低腐蚀防护能力。这些缺陷可通过原位或后处理方法进行密封。本研究比较了二氧化硅颗粒和后碱处理对 AZ31 镁(Mg)合金上形成的 PEO 涂层耐腐蚀性的密封效果。PEO 在含有 2 g/l 纳米颗粒 SiO2 的磷酸盐电解液中以 300 A/m2 的恒定电流密度进行 10 分钟。后碱处理在 0.5 M NaOH 溶液中进行,温度为 80 °C,时间为 30 分钟。使用极化、电化学阻抗光谱和失重测试对耐腐蚀性能进行了评估。二氧化硅颗粒成功地均匀嵌入了 Mg3(PO4)2 涂层,增强了涂层的致密性和稳定性。增强涂层的阻抗模量提高了十倍,腐蚀电流密度降低了。后碱处理提高了耐腐蚀性,但不如 SiO2 增强层高。碱处理试样的阻抗模量提高了五倍,腐蚀电流密度降低了三倍。失重试验一致表明,SiO2 增强涂层在模拟体液中浸泡 14 天后产生的质量损失较小。
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引用次数: 0
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