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A clearer understanding of the dynamic structuring of different natural rubber genotypes on a macroscopic and mesoscopic scale by asymmetrical-flow field-flow fractionation (A4F) analysis 通过非对称流场-流分馏(A4F)分析,在宏观和中观尺度上更清晰地了解不同天然橡胶基因型的动态结构
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-19 DOI: 10.1016/j.polymertesting.2024.108614
Siriluck Liengprayoon , Christine Char , Laurent Vaysse , Frédéric Bonfils
Unlike synthetic elastomers, the structure of natural rubber (NR) evolves (dynamic structuring) and so do its properties during the storage before reaching an industrial mixer. In the rubber industry this is known as storage hardening. NR samples from three genotypes (GT1, RRIM600 and PB235) were subjected to different levels of structuring by varying the structuring time (t) on phosphorus pentoxide (0 < t < 28 h). Storage hardening (ΔP) of the samples was then determined by measuring the increase in Wallace plasticity (P) (macro-scale) and by analyzing their mesostructure (meso-scale) using asymmetrical flow field flow fractionation (A4F). Monitoring ΔP as a function of structuring time revealed a diversity of behaviors specific to the genotype from which the rubber originated. For example, NR samples from genotypes GT1 and PB235 exhibited different kinetics for t < 12 h, an increase in ΔP with structuring time, but reached the same final plateau (t > 12 h). An A4F analysis of the samples was used to quantify the fraction of microaggregates smaller than 1 μm (microgel<1μ). The microgel<1μ rate decreased with structuring time to varying extents depending on the genotype. A very significant negative relationship was found between ΔP and the microgel<1μ rate, indicating that the NR samples that hardened the most contained the lowest microgel<1μ rate, but the highest macrogel rate.
与合成弹性体不同,天然橡胶(NR)的结构会发生变化(动态结构化),在进入工业混炼机之前的储存过程中,其特性也会发生变化。在橡胶工业中,这被称为储存硬化。通过改变五氧化二磷上的结构化时间(t)(0 < t < 28 小时),对三种基因型(GT1、RRIM600 和 PB235)的 NR 样品进行了不同程度的结构化处理。然后通过测量华莱士塑性(P)的增加(宏观尺度)和使用非对称流场流动分馏(A4F)分析样品的中观结构(中观尺度)来确定样品的贮存硬化(ΔP)。通过监测ΔP 与结构化时间的函数关系,可以发现橡胶基因型所特有的各种行为。例如,基因型 GT1 和 PB235 的 NR 样品在 t < 12 小时内表现出不同的动力学,ΔP 随结构化时间的延长而增加,但最终达到相同的高点(t > 12 小时)。样品的 A4F 分析用于量化小于 1 μm 的微团聚体(microgel<1μ)。根据基因型的不同,微凝胶<1μ率随结构化时间的延长而不同程度地降低。ΔP与微凝胶<1μ速率之间存在非常明显的负相关关系,这表明硬化程度最高的 NR 样品所含的微凝胶<1μ速率最低,但大凝胶速率最高。
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引用次数: 0
XPS analysis of damp heat aged and fractured polymer/glass laminates 湿热老化和断裂聚合物/玻璃层压板的 XPS 分析
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-19 DOI: 10.1016/j.polymertesting.2024.108617
Gary Säckl , Gernot M. Wallner , Jiri Duchoslav , Martin Tiefenthaler , David Stifter
Essential for the durability of photovoltaic (PV) modules is the polymeric encapsulant. In addition to the well-established ethylene vinyl acetate copolymers (EVA), polyolefin elastomers (POE) are gaining market relevance. The main objective of this paper was to elucidate the ageing and degradation mechanisms of PV relevant glass laminates based on UV-transparent EVA and POE encapsulants by X-ray photoelectron spectroscopy (XPS).
Special focus was given to the polymer/glass interfaces. Therefore, glass laminates were damp heat aged and debonded by monotonic compressive shear testing. Subsequently, the polymer side of the fractured surfaces was characterized by XPS and Fourier-transform infrared spectroscopy (FTIR). The polar EVA encapsulant revealed more pronounced deterioration than the less polar POE material.
Significant differences were already discernible after 1kh of damp heat exposure. The diffusion of Na ions from the glass substrate into the polymer matrix and the formation of Na salts at the interface were ascertained for EVA and to a less extent also for POE. While EVA laminates failed primarily close to the interface, but still within the EVA material, glass residues were detected on the fractured POE surfaces indicating interface-near glass corrosion and a fracture path propagating back and forth within POE and glass.
聚合物封装材料对光伏(PV)组件的耐用性至关重要。除了应用广泛的乙烯-醋酸乙烯共聚物(EVA)之外,聚烯烃弹性体(POE)也越来越受到市场的重视。本文的主要目的是通过 X 射线光电子能谱(XPS)阐明基于透紫外线 EVA 和 POE 封装剂的光伏相关玻璃层压板的老化和降解机制。因此,对玻璃层压板进行了湿热老化,并通过单调压缩剪切测试使其脱胶。随后,通过 XPS 和傅立叶变换红外光谱(FTIR)对断裂表面的聚合物侧进行了表征。极性 EVA 封装材料比极性较弱的 POE 材料显示出更明显的劣化现象。在 EVA 中,Na 离子从玻璃基质扩散到聚合物基质中,并在界面上形成 Na 盐,在 POE 中也是如此,但程度较轻。EVA 层压板主要在靠近界面的地方失效,但仍在 EVA 材料内部,而在断裂的 POE 表面检测到玻璃残留物,这表明界面附近存在玻璃腐蚀,断裂路径在 POE 和玻璃内部来回传播。
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引用次数: 0
Insights on the polymerization kinetics of non-isocyanate polyurethanes (NIPU) using in situ NMR spectroscopy 利用原位核磁共振光谱深入了解非异氰酸酯聚氨酯 (NIPU) 的聚合动力学
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-19 DOI: 10.1016/j.polymertesting.2024.108615
Anthony Monmagnon , Pierre-Alain Bayle , Florence Flaig , Céline Carpe , Jaouad El Harfi , Renaud Demadrille , Sébastien Rolere
An in situ characterization method using liquid Nuclear Magnetic Resonance (NMR) spectroscopy has been developed to aid the preparation of highly reactive non-isocyanate polyurethanes (NIPUs) from cyclic carbonate aminolysis. Using this methodology, the aminolysis kinetics and the final polymer structure of a model NIPU obtained by reaction of a 5-membered bis-cyclic carbonate (5CC) and 1,4-diaminobutane have been fully investigated, as a function of the type and concentration of the aminolysis catalyst, and the reaction temperature. Several catalysts already reported in NIPUs syntheses, including 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD) and 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), have been compared. The kinetics of the 5CC hydrolysis side reaction was also studied. With an activation energy of 29.7 kJ mol−1, TBD was clearly the most efficient catalyst used, allowing 5CC conversion ratio of up to 100 % using a concentration of 0.35 eq5CC. However, under these experiment conditions, TBD concentration also showed to have a non-negligible influence on the hydrolysis rate, representing between 6 and 14 % of the initial 5CC concentrations, at 353 K. Neither the catalyst or the temperature seemed to affect the polymer structure, with secondary hydroxyl-containing isomer proportions of (70 ± 6) %. Finally, this in situ NMR method is paving the way for rapid screening of innovative catalysts for sustainable NIPU synthesis.
我们开发了一种利用液体核磁共振 (NMR) 光谱进行原位表征的方法,以帮助从环状碳酸酯氨解中制备高活性非异氰酸酯聚氨酯 (NIPU)。利用这种方法,我们充分研究了 5 元双环碳酸酯 (5CC) 与 1,4-二氨基丁烷反应生成的模型 NIPU 的氨解动力学和最终聚合物结构,以及氨解催化剂的类型和浓度以及反应温度对其的影响。对已报道的几种 NIPUs 合成催化剂进行了比较,包括 1,5,7-三氮杂双环[4.4.0]癸-5-烯 (TBD) 和 1,8-二氮杂双环[5.4.0]十一-7-烯 (DBU)。此外,还研究了 5CC 水解副反应的动力学。TBD 的活化能为 29.7 kJ mol-1,显然是最有效的催化剂,在 0.35 eq5CC 的浓度下,5CC 转化率可达 100%。不过,在这些实验条件下,TBD 的浓度对水解率也有不可忽视的影响,在 353 K 的条件下,TBD 的浓度占初始 5CC 浓度的 6% 到 14%。催化剂和温度似乎都不会影响聚合物结构,含仲羟基的异构体比例为 (70 ± 6)%。最后,这种原位核磁共振方法为快速筛选可持续合成 NIPU 的创新催化剂铺平了道路。
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引用次数: 0
Solvent-free synthesis of bio-based non-isocyanate polyurethane (NIPU) with robust adhesive property and resistance to low temperature 无溶剂合成生物基非异氰酸酯聚氨酯 (NIPU),具有良好的粘合性和耐低温性
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-19 DOI: 10.1016/j.polymertesting.2024.108616
Ping Zhang, Hanxiang Guo, Chen Qin, Hao Yuan, Yizhong Cao, Zhe Wang, Chunde Jin
Non-isocyanate polyurethane (NIPU) adhesives represent a cutting-edge advancement in adhesive technology, poised to significantly diminish the dependency on isocyanate-based PU within the industry. In the context of the increasing scarcity of petroleum-based resources and the growing imperative for sustainable environmental practices, the pursuit of a comprehensively sustainable, bio-derived non-isocyanate polyurethane (NIPU) adhesive has swiftly become a pivotal area of interest within the scientific research community. In this study, the cashew phenol cyclic carbonate (CPCC) was synthesized through the addition polymerization process involving cashew phenol glycidyl ether (602A) with carbon dioxide (CO2), followed by a curing step utilizing a diamine extracted from biomass-derived oils to produce bio-based NIPU at ambient temperature. The synthesized NIPU adhesive demonstrated remarkable thermal stability and exceptional adhesion to a variety of substrate materials. Notably, the adhesive showcased superior bonding efficacy at ultra-low temperatures, with steel bonding strength reaching up to 7.78 MPa at -37°C. This study presents an efficient and accelerated synthesis approach for the preparation of bio-based NIPU, offering a significant contribution to the field. Moreover, it provides a valuable reference for future advancements in NIPU adhesive technology, particularly for applications requiring robust bonding at low-temperature environments.
非异氰酸酯聚氨酯(NIPU)粘合剂代表了粘合剂技术的尖端进步,有望显著减少行业内对异氰酸酯基聚氨酯的依赖。随着石油资源的日益稀缺和可持续环境实践的日益迫切,追求全面可持续的生物衍生非异氰酸酯聚氨酯(NIPU)粘合剂已迅速成为科学研究界关注的一个关键领域。本研究通过腰果酚缩水甘油醚(602A)与二氧化碳(CO2)的加成聚合工艺合成了腰果酚环碳酸酯(CPCC),然后利用从生物质油中提取的二胺进行固化,在常温下生产出生物基 NIPU。合成的 NIPU 粘合剂具有显著的热稳定性,对各种基底材料的粘附性也非常出色。值得注意的是,这种粘合剂在超低温条件下显示出卓越的粘合功效,在-37°C时钢材粘合强度高达7.78兆帕。本研究提出了一种高效、快速制备生物基 NIPU 的合成方法,为该领域做出了重要贡献。此外,它还为未来 NIPU 粘合剂技术的发展提供了宝贵的参考,特别是对于需要在低温环境下进行强力粘接的应用。
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引用次数: 0
Char, gas, and action: Transfer of the flame-retardant modes of action in epoxy resins and their fiber-reinforced composites 炭、气体和作用:环氧树脂及其纤维增强复合材料阻燃作用模式的转移
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-15 DOI: 10.1016/j.polymertesting.2024.108610
Maria Jauregui Rozo , Sruthi Sunder , Holger Ruckdäschel , Bernhard Schartel
Flame retardants are often developed for epoxy resins and then transferred into their fiber-reinforced composites with uncertain results. Understanding this transfer in detail represents a critical scientific challenge. This study systematically compares epoxy resins with their glass-fiber reinforced composites, focusing on bisphenol A diglycidyl ether with the hardener dicyandiamide, the flame retardants melamine polyphosphate, ammonium polyphosphate, and silane ammonium polyphosphate, along with inorganic silicate. The research investigates changes in pyrolysis (thermogravimetry), flammability (UL 94, limiting oxygen index), and fire behavior (cone calorimeter) while also examining the flame-retardant modes of action and overall fire performance. The findings reveal that alterations in the amount of fuel, thermal properties, melt flow, and protective layer significantly impact ignition, flammability, and fire load, with a critical reduction in carbonaceous char within the composites preventing intumescence. This study quantifies the effects and provides a fundamental scientific understanding of the complex transfer process of flame retardants from resins to composites, offering essential insights that are of major importance for developing more effective flame-retardant materials.
阻燃剂通常是为环氧树脂开发的,然后转用到纤维增强复合材料中,结果并不确定。详细了解这种转移是一项重要的科学挑战。本研究对环氧树脂及其玻璃纤维增强复合材料进行了系统比较,重点关注双酚 A 二缩水甘油醚、固化剂双氰胺、阻燃剂三聚氰胺聚磷酸盐、聚磷酸铵、硅烷聚磷酸铵以及无机硅酸盐。研究调查了热解(热重仪)、可燃性(UL 94、极限氧指数)和火灾行为(锥形量热仪)的变化,同时还检查了阻燃剂的作用模式和整体防火性能。研究结果表明,燃料量、热性能、熔体流动和保护层的改变会对点火、可燃性和火灾负荷产生重大影响,而复合材料中碳质炭化物的严重减少则会阻止膨胀。这项研究量化了这些影响,并对阻燃剂从树脂到复合材料的复杂转移过程提供了基本的科学认识,为开发更有效的阻燃材料提供了重要的启示。
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引用次数: 0
The Effects of Loading Angles on the Failure of Cross-Ply Notched Bio-Basalt Composites 加载角度对交叉层缺口生物钴复合材料失效的影响
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-11 DOI: 10.1016/j.polymertesting.2024.108609
Zoran Bergant, Roman Šturm, Tomaž Kek, Miroslav Halilovič, Andraž Maček
A cross-ply basalt V-notched butterfly specimens were subjected to pure tension, combined tension-shear, and shear stress-strain state using a modified Arcan test fixture with loading angles from 0° to 90° with 15° increment. Multiaxial stress and strain states were studied using the principal stress and strain ratio, from which the principal angle was determined and used to represent principal states in the gauge section. The quasi-elastic to non-linear transition stresses were determined for each loading angle. In biaxial stress-strain states and pure shear, the deformation and consequently the shear-induced damage start to accumulate significantly. Also, in biaxial stress-strain states between 15°-75°, the shift from tension-shear to pure shear was observed after the transition to the non-linear part of the stress-strain curve. The digital image correlation (DIC) images and microscopic evaluation show that a large extent of damage is the consequence of the shear deformation after the rotation of 0° clamped fibres, while the 90° fibres maintained their original straight form. In off-axis tests, the principal strain axis rotates towards the weakest material axis even at small off-axis angles. This causes a transition from a tension-shear biaxial state in the linear loading part to shear in the non-linear part, leading to irreversible damage beyond the transition point.
使用改进的 Arcan 试验夹具,以 15° 为增量,从 0° 到 90° 的加载角度,对交叉层状玄武岩 V 型缺口蝶形试样进行了纯拉伸、拉伸-剪切组合和剪切应力-应变状态试验。使用主应力和应变比研究多轴应力和应变状态,从中确定主角,并用它来表示量具截面中的主状态。确定了每个加载角度的准弹性到非线性过渡应力。在双轴应力-应变状态和纯剪切状态下,变形和剪切引起的损伤开始显著累积。此外,在 15°-75° 之间的双轴应力-应变状态下,在应力-应变曲线的非线性部分过渡之后,观察到了从拉伸-剪切到纯剪切的转变。数字图像相关(DIC)图像和显微镜评估表明,0°夹持纤维旋转后的剪切变形造成了很大程度的损坏,而 90°夹持纤维则保持了原有的直线形态。在偏轴试验中,即使偏轴角度很小,主应变轴也会向最薄弱的材料轴旋转。这导致从线性加载部分的拉伸-剪切双轴状态过渡到非线性部分的剪切状态,从而导致过渡点以外的不可逆损坏。
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引用次数: 0
Ultra-strength and anti-freezing zwitterionic hydrogels with high ion conductivity: Effect of the hydrophobic monomer in hydrogels mechanical properties 具有高离子传导性的超强度抗冻齐聚物水凝胶:疏水单体对水凝胶机械性能的影响
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-10 DOI: 10.1016/j.polymertesting.2024.108607
Hatam Najafi Fath Dehghan , Amir Abdolmaleki , Mehdi Pourahmadi , Sepideh Hozori , Ehsan Gaeini , Seyed Younes Mousavi , Amir-Reza Arvaneh , Mehdi Sadat-Shojai
Zwitterionic hydrogels have emerged as a promising option due to their remarkable ionic conductivity. However, these hydrogels often suffer from poor mechanical properties due to their super hydrophilicity. Herein, we propose the use of a rigid aryl imidazolium monomer (AIm) for crosslinking with poly(vinyl alcohol) (PVA) to create a unique zwitterion hydrogel. Chlorosulfonic acid acts as an agent to introduce anionic groups, facilitating the transfer of Zn2⁺ ions in zwitterionic hydrogel. We achieve extraordinary mechanical properties by incorporating an optimal amount of AIm into the PZW2 hydrogel (tensile stress 0.9 MPa and stretch 1400 %). Above all, the PZW2 hydrogel exhibits remarkable resistance to freezing, remaining unfrozen even at up to −80 °C. This anti-freezing property is attributed to the cation-dipole interactions and the presence of ZnCl2, effectively preventing water from freezing within the hydrogel structure. Furthermore, the PZW2 hydrogel demonstrates a high ionic conductivity of 4.34 S m−1 at room temperature. This can be attributed to the presence of anionic and cationic charges within the PZW2 hydrogel, which facilitates the transfer of ions through a hopping mechanism. The PZW2 hydrogel demonstrates better performance compared to most antifreeze conductive hydrogels. At −20 °C, it achieves an impressive ionic conductivity of 2.73 S m−1 and retains outstanding mechanical characteristics with a stretchability of 1000 %. Ultimately, the PZW2 hydrogel demonstrates a sensitive response performance with a gauge factor of 1.59, making it highly suitable for potential sensor applications.
由于具有显著的离子传导性,两性离子水凝胶已成为一种很有前景的选择。然而,这些水凝胶往往因其超亲水性而具有较差的机械性能。在此,我们建议使用刚性芳基咪唑单体(AIm)与聚乙烯醇(PVA)交联,从而制造出一种独特的齐聚物水凝胶。氯磺酸可作为引入阴离子基团的媒介,促进 Zn2⁺离子在齐聚物水凝胶中的转移。通过在 PZW2 水凝胶中加入最适量的 AIm,我们获得了非凡的机械性能(拉伸应力为 0.9 兆帕,拉伸率为 1400%)。最重要的是,PZW2 水凝胶具有卓越的抗冻性,即使在零下 80 °C 的环境中也不会冻结。这种抗冻特性归功于阳离子-偶极相互作用和 ZnCl2 的存在,从而有效地防止了水凝胶结构中的水结冰。此外,PZW2 水凝胶在室温下的离子电导率高达 4.34 S m-1。这可归因于 PZW2 水凝胶中存在阴离子和阳离子电荷,从而通过跳跃机制促进了离子的转移。与大多数防冻导电水凝胶相比,PZW2 水凝胶具有更好的性能。在零下 20 °C,它的离子导电率达到了惊人的 2.73 S m-1,并保持了出色的机械特性,伸展性高达 1000%。最终,PZW2 水凝胶的灵敏响应性能达到了 1.59,非常适合传感器的潜在应用。
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引用次数: 0
Rheological analysis of network structure of raw natural rubber prepared by different processing techniques 不同加工技术制备的天然生橡胶网络结构的流变学分析
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-10 DOI: 10.1016/j.polymertesting.2024.108608
Rui Wang , Lusheng Liao , Pengfei Zhao , Heping Yu , Fuquan Zhang , Gaorong Li , Zheng Peng
The performance of raw natural rubber (NR) is dominated by its network structure, particular the levels of long chain branching (LCB) and entanglement. Here, three type of raw rubbers were prepared using different processing methods for commercial grade NRs. Linear and nonlinear viscoelastic behaviors, as well as stress relaxation, were analyzed to access their network structures. The third relative harmonic, phase angle, and first to second quarter-period integral ratio of stress curve were utilized as indicators for the nonlinearity of samples. By combining these values with flow activation energy and characteristic times, it can be confirmed that naturally coagulated NR showed higher elasticity than acid-coagulated NR due to high levels of LCB and entanglement, and hot air drying could lead to chain degradation. These findings correlated with molecular weight parameters, gel content and Mooney viscosity results. This research establishes a method for monitoring raw NR quality and predicting its properties.
天然橡胶(NR)生胶的性能主要取决于其网络结构,尤其是长链分支(LCB)和缠结程度。本文采用不同的加工方法制备了三种商用级天然橡胶生胶。分析了它们的线性和非线性粘弹行为以及应力松弛,以了解它们的网络结构。应力曲线的三次相对谐波、相位角和第一至第二四分之一周期积分比被用作样品非线性的指标。通过将这些值与流动活化能和特征时间相结合,可以确认自然凝固的 NR 由于高水平的 LCB 和缠结而比酸凝固的 NR 表现出更高的弹性,而热空气干燥可能会导致链降解。这些发现与分子量参数、凝胶含量和门尼粘度结果相关。这项研究建立了一种监测未加工 NR 质量和预测其特性的方法。
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引用次数: 0
Flexible and innovative PVA/ZrO2/g-C3N4/CNT nanocomposites film for optoelectronic applications 用于光电应用的柔性创新 PVA/ZrO2/g-C3N4/CNT 纳米复合薄膜
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-05 DOI: 10.1016/j.polymertesting.2024.108604
Majed Alshammari
This study successfully prepared polyvinyl alcohol (PVA) polymer films doped with ZrO2/(g-C3N4/CNT) nanofillers using the solution casting technique. The crystal structure of the nanocomposite films was characterized by X-ray diffraction (XRD), revealing the semi-crystalline nature of PVA and an average ZrO2 crystallite size of 13.17 nm. Fourier-transform infrared (FTIR) spectroscopy confirmed the chemical composition and functional groups present in the nanocomposites. Scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) analysis showed uniform dispersion of the nanofillers without noticeable phase separation, with EDX confirming the successful incorporation of ZrO2, g-C3N4, and CNT into the PVA matrix. X-ray photoelectron spectroscopy (XPS) further validated the elemental composition and chemical states, indicating the presence of carbon, oxygen, nitrogen, and zirconium. Optical analysis demonstrated that increasing ZrO2/(g-C3N4/CNT) content reduced the direct and indirect band gaps from 5.41 eV to 5.25 eV and from 5.18 eV to 4.92 eV, respectively. In addition, the single-oscillator energy (E0) and dispersion energy (Ed) increased, while the static refractive index (n0) decreased. Improvements were also observed in linear optical susceptibility (χ(1)) and third-order nonlinear optical susceptibility (χ(3)), enhancing the polarizability of the polymer molecules. These results indicate that PVA films doped with ZrO2/(g-C3N4/CNT) hold promise for optoelectronic applications due to their enhanced optical properties.
本研究采用溶液浇铸技术成功制备了掺杂有 ZrO2/(g-C3N4/CNT) 纳米填料的聚乙烯醇(PVA)聚合物薄膜。X 射线衍射 (XRD) 表征了纳米复合薄膜的晶体结构,结果表明 PVA 为半结晶性质,ZrO2 的平均结晶尺寸为 13.17 nm。傅立叶变换红外光谱(FTIR)证实了纳米复合材料中的化学成分和官能团。扫描电子显微镜(SEM)和能量色散 X 射线(EDX)分析表明,纳米填料均匀分散,没有明显的相分离现象。X 射线光电子能谱(XPS)进一步验证了元素组成和化学状态,表明存在碳、氧、氮和锆。光学分析表明,ZrO2/(g-C3N4/CNT)含量的增加使直接和间接带隙分别从 5.41 eV 降至 5.25 eV 和从 5.18 eV 降至 4.92 eV。此外,单振子能量(E0)和色散能量(Ed)增加,而静态折射率(n0)降低。线性光学感度(χ(1))和三阶非线性光学感度(χ(3))也得到了改善,从而提高了聚合物分子的极化能力。这些结果表明,掺杂 ZrO2/(g-C3N4/CNT) 的 PVA 薄膜因其增强的光学特性而有望用于光电应用。
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引用次数: 0
Characterization of the in-situ degradation process of P3HT:PCBM based on hyperspectral and neural networks 基于高光谱和神经网络的 P3HT:PCBM 原位降解过程表征
IF 5 2区 材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Pub Date : 2024-10-04 DOI: 10.1016/j.polymertesting.2024.108606
Yang Wang , Zhao Ding , Junli Li , Ting Yang , Jianfeng Chen , Lifeng Bian , Chen Yang
In situ online observation of surface morphology during degradation processes is of paramount importance for exploring the stability of organic photovoltaic materials. In this study, we designed an in situ online characterization system based on hyperspectral and neural network technologies, and observed the degradation processes of P3HT:PCBM thin film materials. The system is capable of collecting hyperspectral image data from 101 channels within the 400–700 nm wavelength range for characterizing detailed surface features of materials. Additionally, to automate the processing of hyperspectral image data, we designed a spectral image segmentation algorithm based on neural networks and proposed a foreground attention mechanism to improve the segmentation accuracy of the algorithm. The experimental results indicate that the system can achieve high spectral characterization of P3HT:PCBM thin film materials and automate image data processing through artificial intelligence algorithms, with an image segmentation accuracy of 99.62 %. Furthermore, owing to the higher spectral resolution of this system and its computer-assisted analysis capabilities for material image data, not only are the in-situ variations in size, density, and formation rate of aggregates formed during the thermal degradation process of P3HT:PCBM thin film materials experimentally analyzed, but also the fluorescence changes at the edges of aggregates during the photodegradation process are revealed. The reliable code can be found at the following link: https://github.com/HyperSystemAndImageProc/IONFMDP-UHHNN.
原位在线观测降解过程中的表面形态对于探索有机光伏材料的稳定性至关重要。在本研究中,我们设计了一种基于高光谱和神经网络技术的原位在线表征系统,并观测了 P3HT:PCBM 薄膜材料的降解过程。该系统能够从 101 个通道收集 400-700 纳米波长范围内的高光谱图像数据,用于表征材料的详细表面特征。此外,为了自动处理高光谱图像数据,我们设计了一种基于神经网络的光谱图像分割算法,并提出了一种前景关注机制,以提高算法的分割精度。实验结果表明,该系统可以实现 P3HT:PCBM 薄膜材料的高光谱表征,并通过人工智能算法实现图像数据的自动化处理,图像分割准确率达到 99.62 %。此外,由于该系统具有较高的光谱分辨率和对材料图像数据的计算机辅助分析能力,不仅能对 P3HT:PCBM 薄膜材料热降解过程中形成的聚集体的尺寸、密度和形成率的原位变化进行实验分析,还能揭示光降解过程中聚集体边缘的荧光变化。可靠的代码见以下链接:https://github.com/HyperSystemAndImageProc/IONFMDP-UHHNN。
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Polymer Testing
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