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Synthesis and photo-initiated radical polymerization of methacrylates derived from bio-based ω-hydroxycarboxylic acids 生物基ω-羟基羧酸衍生甲基丙烯酸酯的合成与光引发的自由基聚合反应
Pub Date : 2024-03-15 DOI: 10.1002/appl.202300124
Markus Heinz, Maximilian Kepkow, Bernd Strehmel, Veronika Strehmel

The bio-based methacrylates 9-(methacryloyloxy)-10,18-dihydroxyoctadecanoic acid/9,18-dihydroxy-10-(methacryloyloxy)octadecanoic acid isomer mixture and 22-methacryloyloxydocosanoic acid were synthesized from 9,10-epoxy-18-hydroxyoctadecanoic acid and 22-hydroxydocosanoic acid. The white crystalline 9,10-epoxy-18-hydroxyoctadecanoic acid and cream-colored 22-hydroxydocosanoic acid were isolated from both the bark of Betula pendula and cork of Quercus suber after extraction of the milled plant materials with methanol, treating the insoluble residues with 2-propanole containing suspended sodium hydroxide, application of a working up procedure developed in this work for the resulting mixture, and purification of the products obtained. The new bio-based methacrylates show higher reactivity in the photoinitiated polymerization in comparison with the commercial laurylmethacrylate as detected by photo-differential scanning calorimetry (DSC). For comparison, traditional free radical polymerization of the new bio-based methacrylates was carried out in dimethylsulfoxide using 2,2'-azobis-(2-propionitrile) as initiator. Furthermore, the quantitative conversion of the bio-based monomers during the photoinitiated polymerization makes these bio-based monomers interesting for application in coatings. As expected, the photopolymer made from the 9-(methacryloyloxy)-10,18-dihydroxyoctadecanoic acid/9,18-dihydroxy-10-(methacryloyloxy)octadecanoic acid isomer mixture is amorphous. Interestingly, the photopolymer made from the 22-methacryloyloxydocosanoic acid contains crystalline structures as detected by DSC investigation.

由 9,10-环氧-18-羟基十八烷酸和 22-羟基二十二酸合成了生物基甲基丙烯酸酯 9-(甲基丙烯酰氧基)-10,18-二羟基十八烷酸/9,18-二羟基-10-(甲基丙烯酰氧基)十八烷酸异构体混合物和 22-甲基丙烯酰氧基二十二酸。用甲醇萃取磨碎的植物材料,用含有悬浮氢氧化钠的 2-丙醇处理不溶性残留物,对得到的混合物采用本研究开发的加工程序,并对得到的产品进行纯化,然后从桦树和柞树的树皮中分离出白色结晶的 9,10-epoxy-18-hydroxyoctadecanoic acid 和乳白色的 22-hydroxydocosanoic acid。与商用十二烷基甲基丙烯酸酯相比,新的生物基甲基丙烯酸酯在光引发聚合中显示出更高的反应活性,这是由光致电导率扫描仪检测到的。为了进行比较,使用 2,2'-偶氮双(2-丙腈)作为引发剂,在二甲基亚砜中对新型生物基甲基丙烯酸酯进行了传统的自由基聚合。此外,生物基单体在光引发聚合过程中的定量转化使得这些生物基单体有望应用于涂料。不出所料,由 9-(甲基丙烯酰氧基)-10,18-二羟基十八烷酸/9,18-二羟基-10-(甲基丙烯酰氧基)十八烷酸异构体混合物制成的光聚合物是无定形的。有趣的是,由 22-甲基丙烯酰氧基二十二酸制成的光聚合物含有结晶结构,这是由 DSC 研究检测到的。本文受版权保护。
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引用次数: 0
Optimizing the series cascade control structure for nonminimum phase system regulation 优化非最小相位系统调节的串联级联控制结构
Pub Date : 2024-03-06 DOI: 10.1002/appl.202300051
Ashish Kumar Singhal, Manish Yadav, Vijay Yadav, Jyoti Deshmukh, Manish Billore, Hirak Mazumdar

This work elucidates the control of integrating a nonminimum phase system via a series cascade scheme with fractional-order P.I. (Proportional–Integral) plus D (Derivative) controller. The traditional Internal Model Control (IMC) is adopted for inner loop controller design. The feedback D controller is synthesized with the outer loop process model, showing the proposed work's universality. The outer loop controller is suggested in the IMC framework after the accountability of fractional-filter and inverse response compensator. This combination is revealed to enhance performance without compromising robustness. The Riemann sheet principle is explored to compute the stability of the suggested controller. The sensitivity analysis has asserted the robustness. More importantly, the optimal value of controller settings is achieved via the Teaching Learning Based Optimization (TLBO) algorithm. This TLBO algorithm uses an objective function that minimizes Integral Square Error. Two illustrative problems are utilized to examine the recommended control structure's virtue.

本研究阐明了通过分数阶 P.I.(比例-积分)加 D(微分)控制器的串联级联方案对非最小相位系统进行集成控制的问题。内环控制器设计采用了传统的内部模型控制(IMC)。反馈 D 控制器与外环过程模型合成,显示了所提议工作的通用性。在 IMC 框架中,建议采用分式滤波器和反响应补偿器。结果表明,这种组合能在不影响稳健性的情况下提高性能。利用黎曼表原理计算了建议控制器的稳定性。灵敏度分析证明了其稳健性。更重要的是,控制器设置的最佳值是通过基于教学学习的优化(TLBO)算法实现的。该 TLBO 算法使用的目标函数是最小化积分平方误差 (ISE)。本文受版权保护。本文受版权保护,保留所有权利。
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引用次数: 0
Leveraging wastewater surveillance to actively monitor Covid-19 community dynamics in rural areas with reduced reliance on clinical testing 利用废水监测积极监测农村地区 Covid-19 群落动态,减少对临床检测的依赖
Pub Date : 2024-03-05 DOI: 10.1002/appl.202400012
Michelle M. Jarvie, Thu N. T. Nguyen, Benjamin Southwell, Derek Wright

The prevalence of coronavirus disease 2019 (Covid-19) in the community has become more difficult to gauge utilizing clinical testing due to a decrease in reported test results stemming from the availability of at-home test kits and a reduction in the number of cases seeking medical treatment. The purpose of this study was to examine the trend of diminishing correlation between reported clinical cases of Covid-19 and wastewater-based surveillance epidemiological data as home testing became available in the Eastern Upper Peninsula of Michigan. Wastewater grab samples were collected weekly from 16 regional locations from June 2021 to December 2022. Samples were analyzed for severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) N1 and N2 viral particles using reverse transcriptase digital droplet polymerase chain reaction (RT ddPCR). N1 and N2 gene copies were correlated with clinical cases. The t test was used to determine the correlation deterioration point. Clinical cases postdeterioration were calculated for high-correlated predeterioration locations using linear regression. Correlation between the wastewater-based surveillance of SARS-CoV-2 and reported clinical cases deteriorated after February 1, 2022. This corresponds with the timeframe in which commercially available at-home test kits became available in the United States. The increase in at-home testing for SARS-CoV-2 likely contributed to the decrease in reported clinical positive tests in early 2022, providing an unrealistic picture of the presence of Covid-19 in the community. As measures to reduce exposure such as personal masking, clinical testing, social isolating, and quarantining continue to decline, wastewater surveillance for the presence of SARS-CoV-2 may be the best method for public health professionals to remain aware of virus dynamics in localized regions. Time-series modeling adds another layer of information when clinical data is unobtainable or underreported.

COVID-19 在社区中的流行程度越来越难以通过临床检测来衡量,原因是家庭检测试剂盒的出现导致报告的检测结果减少,以及寻求医疗治疗的病例数量减少。本研究的目的是考察密歇根州东部上半岛地区随着家庭检测的普及,COVID-19 临床病例报告与基于废水的监测流行病学数据之间相关性降低的趋势。2021 年 6 月至 2022 年 12 月期间,每周从 16 个地区采集废水样本。使用逆转录酶数字液滴聚合酶链反应(RT ddPCR)分析样本中的 SARS-CoV-2 N1 和 N2 病毒颗粒。N1 和 N2 基因拷贝与临床病例相关。采用 t 检验确定相关性恶化点。使用线性回归法计算恶化前高相关性地点恶化后的临床病例。2022 年 2 月 1 日之后,基于废水的 SARS-CoV-2 监测与报告的临床病例之间的相关性下降。这与美国商业化家庭检测试剂盒上市的时间相吻合。SARS-CoV-2 居家检测的增加很可能导致 2022 年初报告的临床检测阳性病例的减少,从而提供了社区中存在 Covid-19 的不真实情况。随着个人遮蔽、临床检测、社会隔离和检疫等减少接触的措施不断减少,对 SARS-CoV-2 的存在进行废水监测可能是公共卫生专业人员了解局部地区病毒动态的最佳方法。当临床数据无法获得或报告不足时,时间序列模型可提供另一层信息。本文受版权保护。
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引用次数: 0
Narrowing lab-to-market gaps: Device innovations in fuel generation, solar-cell, and photodetection 缩小实验室到市场的差距:燃料发电、太阳能电池和光电检测领域的设备创新
Pub Date : 2024-03-05 DOI: 10.1002/appl.202300109
Sukanta Nandi, Raaghesh Vijayan, Manjeet Chhetri

Academic translational research efforts to industry are often an underlying sought-after goal among various researchers. Through the interchanges of research endeavors between academia-industry, great innovations can/has been achieved that cater to the real-world application by bridging “industrially relevant” problem solving with pursuing fundamental studies. It is pertinent that most of the studies from university-level research works may not translate into demonstrable market products due to various reasons. Funding support, individual researcher goals, socioeconomic factors, and most importantly the technical know-how of generating revenue strategies for startups, are a few of the factors that have slowed the pace of collaborative efforts. However, we believe that the most crucial component is the identification of the critical parameters that solve long-standing problems that hinder the scale-up of the lab scale research into marketable products considering the techno-economic analysis. To illustrate this, we take the three most relevant examples of devices for fuel generation, devices to utilize solar radiation, and devices for detection and other related applications. In this perspective, we provide an in-depth case study of each of these critical parameters to comment on the direction of research avenues that can serve as step-stones for the commercialization of university-level lab research studies.

面向产业的学术转化研究工作往往是不同研究人员追求的基本目标。通过学术界与产业界之间的研究工作交流,在解决 "与产业相关 "的问题与开展基础研究之间架起了一座桥梁,从而能够/已经取得了巨大的创新成果,满足了现实世界的应用需求。与此相关的是,由于各种原因,大学研究工作中的大多数研究可能无法转化为可证实的市场产品。资金支持、研究人员的个人目标、社会经济因素,以及最重要的初创企业创收战略的技术诀窍,都是放慢合作步伐的几个因素。然而,我们认为,最关键的因素是要确定关键参数,以解决长期存在的问题,这些问题阻碍了实验室规模研究向市场化产品的扩展,同时还要考虑到技术经济分析。为了说明这一点,我们以燃料生产设备、太阳辐射利用设备和检测设备及其他相关应用设备这三个最相关的设备为例进行说明。从这一角度出发,我们对每个关键参数都进行了深入的案例研究,以评述可作为大学实验室研究成果商业化基石的研究途径的方向。本文受版权保护。
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引用次数: 0
Epitaxial silicon transition zone measurements by spreading resistance profiling and Fourier transform infrared reflectometry 利用展阻剖面法 (SRP) 和傅立叶变换红外反射仪测量外延硅过渡区
Pub Date : 2024-03-01 DOI: 10.1002/appl.202300146
Eszter E. Najbauer, Lucza Sinkó, Szilvia Biró, Zsolt Durkó, Peter Basa

Silicon epitaxy is an essential building block in the manufacturing of complementary metal-oxide semiconductor (CMOS) devices. Accurate determination of epitaxial layer thickness is indispensable for a uniform and reproducible process. In this paper, we compare thickness values of the transition zone (TZ) in silicon epitaxial wafers obtained by two of Semilab's production-compatible electrical and optical characterization techniques: Fourier-transform infrared (FTIR) reflectometry and spreading resistance profiling (SRP). We demonstrate a high correlation between TZ thicknesses obtained from the optical modeling of FTIR reflectance spectra and SRP profiles. The dependence of TZ thickness change on the high-temperature annealing steps is also examined. FTIR reflectometry thus offers a quick, contactless alternative for obtaining structural parameters of an epitaxial layer, and these values can be well matched to those given by SRP.

硅外延是制造互补金属氧化物半导体(CMOS)器件的重要组成部分。外延层厚度的精确测定对于实现均匀、可重复的工艺是不可或缺的。在本文中,我们比较了通过 Semilab 两种与生产兼容的电气和光学表征技术获得的硅外延片过渡区的厚度值:傅立叶变换红外(FTIR)反射仪和展阻曲线(SRP)。我们证明了通过傅立叶变换红外反射光谱光学建模获得的过渡区厚度与 SRP 曲线之间的高度相关性。我们还研究了过渡区厚度变化与高温退火步骤的关系。因此,傅立叶变换红外反射仪为获得外延层的结构参数提供了一种快速、非接触式的替代方法,而且这些参数值与 SRP 所给出的参数值非常匹配。本文受版权保护。
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引用次数: 0
Alternative during-growth chlorination of sputtered CdTe films and their implementation as activating layers in CdS/CdTe solar cells 溅射碲化镉薄膜在生长过程中的替代氯化工艺及其在 CdS/CdTe 太阳能电池中作为激活层的应用
Pub Date : 2024-02-28 DOI: 10.1002/appl.202300143
Abraham Israel Calderón-Martínez, Omar Jiménez-Sandoval, Francisco Rodríguez-Melgarejo, Martín Adelaido Hernández-Landaverde, Francisco Javier Flores-Ruiz, Sergio Joaquín Jiménez-Sandoval

Cadmium telluride is an efficient light absorbing material successfully used in solar cell technology. The efficiency of such photovoltaic devices is strongly dependent on post-deposition thermal treatments in the presence of chlorine. The benefits of this process on the absorbing layer include removal of intragrain defects, grain growth enhancement, and grain boundaries passivation. The absorber chlorination is a crucial step for which CdCl2 is the most common choice. Its use, however, has been overshadowed by the toxicity of Cd- and Cl-containing vapors and residues. In this work, chlorine was incorporated in CdTe films during growth using sputtering targets with different chloride compounds: CdCl2, TeCl4, BaCl2, CaCl2, or LiCl. After characterizing these films, CdTe:CdCl2 and CdTe:TeCl4 were selected as feasible absorbers for testing their performance in photovoltaic devices. Efficiencies near 7% were obtained in as-grown unoptimized cells in which the absorber consisted of two layers: pristine CdTe and CdTe:CdCl2 or CdTe:TeCl4. The chlorinated layers acted as Cl sources for the adjacent CdTe and CdS, which produced a homogeneous distribution of chlorine throughout the cell. In the during-growth activating-layer (DG-AL) method used here, the chlorine diffusion during growth had a doping effect, passivated grain boundaries and defects, improved the back contact characteristics by reducing the CdTe work function, and lowered the pinhole formation probability by producing a compact chlorinated CdTe layer.

碲化镉是一种高效的光吸收材料,已成功应用于太阳能电池技术。这种光伏设备的效率在很大程度上取决于氯存在下的沉积后热处理。这种工艺对吸收层的好处包括消除晶粒内缺陷、增强晶粒生长和晶界钝化。吸收层氯化是最常用的关键步骤。然而,由于含 Cd 和 Cl 的蒸气和残留物的毒性,它的使用已经黯然失色。在这项工作中,使用不同氯化物的溅射靶材在碲化镉薄膜生长过程中加入了氯:CdCl2、TeCl4、BaCl2、CaCl2 或 LiCl。在对这些薄膜进行表征后,CdTe:CdCl2 和 CdTe:TeCl4 被选为可行的吸收体,用于测试它们在光伏设备中的性能。在未优化的电池中,吸收剂由两层组成:原始碲化镉和碲化镉:CdCl2 或碲化镉:TeCl4。氯化层是相邻碲化镉和硒化镉的氯源,从而在整个电池中形成均匀的氯分布。在本文使用的生长过程中激活层(DG-AL)方法中,生长过程中的氯扩散具有掺杂效应,钝化了晶界和缺陷,通过降低碲化镉功函数改善了背接触特性,并通过产生致密的氯化碲化镉层降低了针孔形成概率。本文受版权保护。
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引用次数: 0
Mechanical behavior of bio-inspired composites made of co-continuous geopolymer and 3D-printed polymer 由共连续土工聚合物和 3d 印刷聚合物制成的生物启发复合材料的力学性能
Pub Date : 2024-02-27 DOI: 10.1002/appl.202300097
Siyuan Pang, Mahmoud A. Mahrous, Ana Carolina Constancio Trindade, Andrij Kozych, Nupur Kale, Waltraud M. Kriven, Iwona Jasiuk

Geopolymers (GPs) are emerging, low-density ceramic materials that are simple to manufacture, with high elastic modulus and strength, albeit with low toughness. Fiber reinforcements have been used to achieve varied ductile behaviors, but little is known about the GP addition to polymeric frame structures. Thus, drawing inspiration from the nanostructure of bones, this paper investigated an interpenetrating, co-continuous composite consisting of a GP as the stiff but brittle phase, and a 3D-printed polymer (PA12 White) as the soft and deformable phase. The composite mechanical properties and failure modes were studied experimentally using uniaxial compression and four-point bending tests. The co-continuous network constrained brittle cracking within the GP and reduced strain localization in the polymer. The results showed that the composite had higher strength (56.11 ± 2.12 MPa) and elastic modulus (6.08 ± 1.37 GPa) than the 3D-printed polymer and had higher toughness (5.98 ± 0.24 MJ/mm3) than the GP for the specific geometries examined. The shape effect study demonstrated that cubic structures had higher elastic modulus and strength but at the expense of lower toughness when compared to rectangular prism structures. The study of scale effects indicated that increasing the number of periodic unit cells while maintaining consistent bulk dimensions led to augmented strength and toughness, albeit without statistically significant alterations in elastic modulus. Thus, this paper presents an experimental realization of a novel, bio-inspired, interpenetrating, GP–polymer composite design, offering improved strength and toughness. It also provides valuable insights into the shape and size effects on the mechanical properties of this new composite.

土工聚合物是新兴的低密度陶瓷材料,制造简单,弹性模量和强度高,但韧性低。纤维增强材料已被用于实现各种韧性行为,但人们对聚合物框架结构中添加土工聚合物的情况知之甚少。因此,本文从骨骼的纳米结构中汲取灵感,研究了一种互穿共连续复合材料,该复合材料由土工聚合物(作为刚性脆性相)和三维打印聚合物(PA12 White)(作为软性可变形相)组成。通过单轴压缩和四点弯曲试验对该复合材料的机械性能和破坏模式进行了实验研究。共连续网络限制了土工聚合物内部的脆性开裂,并减少了聚合物中的应变局部化。结果表明,在特定几何形状下,复合材料的强度(56.11 ± 2.12 MPa)和弹性模量(6.08 ± 1.37 GPa)均高于三维打印聚合物,韧性(5.98 ± 0.24 MJ/mm3)也高于土工聚合物。形状效应研究表明,与矩形棱柱结构相比,立方体结构具有更高的弹性模量和强度,但韧性较低。对尺度效应的研究表明,在保持体积尺寸一致的情况下,增加周期性单元格的数量可提高强度和韧性,尽管在统计上弹性模量没有显著变化。因此,本文通过实验展示了一种新颖的受生物启发的互渗土工聚合物-聚合物复合材料设计,该设计具有更高的强度和韧性。本文受版权保护。本文受版权保护,保留所有权利。
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引用次数: 0
Multifunctional aptamer grafted targeted nano-drugs execute molecular cross-talks with cancer cells 多功能适配体接枝靶向纳米药物与癌细胞发生分子交叉作用
Pub Date : 2024-02-20 DOI: 10.1002/appl.202300115
Sounik Manna, Rumi Mahata, Surya K. Dey, Angsuman Das Chaudhuri, Sujata M. Choudhury

The biggest obstacles in treating cancer with traditional chemotherapy are unpleasant side effects and drug resistance. A growing amount of interest has been exhibited in using aptamers as target ligands for targeted cancer therapy and specific cancer cell identification due to their distinct benefits. Aptamer-conjugated nano-materials have recently provided new prospects in cancer treatment with their improved therapeutic efficacy and capability of reducing toxicity. Consequently, they are not perceived as alien substances our body, which allows their comfortable acceptance. Several tumor markers such as nucleolin, mucin, and the epidermal growth factor receptor can be effectively recognized by aptamers. In addition, glycoproteins on the surface of tumor cells can be recognized using aptamers. So surface modification of drug by aptamer are accomplished for enhanced tumor-specific recognition by which drug-specific accretion, internalization, and drug retention in tumors increased through specific ligand-mediated interactions and thus therapeutic index is increased. Here, we highlight some promising classes of aptamer-conjugated nanoparticles for the specific recognition of cancer cells and targeted drug delivery and the molecular mechanism and immunomodulatory regulation of these aptamer have been focused.

传统化疗治疗癌症的最大障碍是令人不快的副作用和耐药性。由于其独特的优势,越来越多的人开始关注使用适配体作为靶配体来进行癌症靶向治疗和特异性癌细胞识别。最近,适配体结合的纳米材料因其更好的疗效和减毒能力,为癌症治疗提供了新的前景。因此,它们不会被认为是人体内的外来物质,因而可以被人们轻松接受。一些肿瘤标志物,如核蛋白、粘蛋白和表皮生长因子受体,都能被适配体有效识别。此外,肿瘤细胞表面的糖蛋白也能被适配体识别。因此,通过适配体对药物进行表面修饰可增强对肿瘤的特异性识别,从而通过配体介导的特异性相互作用增加药物在肿瘤中的特异性吸附、内化和保留,从而提高治疗指数。本文受版权保护。本文受版权保护,未经许可不得转载。
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引用次数: 0
Rapid tooling for rubber extrusion molding by digital light processing 3D printing with dual curable vitrimers 利用数字光处理 3D 打印技术和双固化玻璃缸实现橡胶挤压成型的快速模具制造
Pub Date : 2024-02-19 DOI: 10.1002/appl.202300133
Rita Höller, Katja Hrbinič, David Reisinger, Walter Alabiso, Stephan Schuschnigg, Mathias Fleisch, Christoph Waly, Elisabeth Rossegger, Sandra Schlögl

For the manufacture of extrusion dies, three-dimensional (3D) printing with photopolymers offers numerous advantages including flexibility, high surface quality, decent build speed, low costs and a reduced amount of waste. However, the majority of photocurable resins used in vat photopolymerization 3D printing rely on acrylates, which entail 3D-printed objects with poor mechanical properties. In particular, the high brittleness limits their application in rapid tooling, for which tough materials with high glass transition temperatures (Tg) are required. In the present study, we highlight the use of dual curable acrylate-epoxy resins with dynamic covalent bonds for the direct fabrication of extrusion dies. During digital light processing (DLP) 3D printing the acrylate network is formed, whose toughness and thermal stability are significantly enhanced by the thermoactivated formation of a second network. By following a postbaking procedure, aminoglycidiyl monomers are cured with an anhydride hardener bearing bulky norbornene groups yielding interpenetrating polymer networks with a Tg > 100°C. The tertiary amine groups present in the structure of the aminoglycidyl derivatives do not only accelerate the ring-opening reaction but also act as internal catalysts and activate bond exchange reactions between free –OH groups and ester moieties available in the photopolymer. This is confirmed by rheometer studies showing a distinctive stress relaxation at elevated temperature and giving rise to a possible reprocessability of the 3D-printed dies. With a selected resin formulation, a set of dies is printed by DLP 3D printing, with which a highly filled rubber compound is successfully extruded. The results clearly show that dual curable resins with dynamic covalent bonds are a promising class of material for rapid tooling and pave the way towards a customized and convenient fabrication of extrusion dies for rubber processing.

对于挤压模具的制造,使用光聚合物进行三维打印具有许多优势,包括灵活性、高表面质量、适当的构建速度、低成本和减少废料量。然而,大桶光聚合三维打印中使用的大多数光固化树脂都依赖于丙烯酸酯,这导致三维打印物体的机械性能较差。特别是,高脆性限制了它们在快速模具中的应用,而快速模具需要具有高玻璃化转变温度(Tg)的坚韧材料。在本研究中,我们重点介绍了使用具有动态共价键的双固化丙烯酸酯-环氧树脂直接制造挤压模具的方法。在数字光处理 3D 打印过程中,丙烯酸酯网络形成,通过热激活形成第二个网络,其韧性和热稳定性显著增强。通过后烘烤程序,氨基缩水甘油酯单体与带有大块降冰片烯基团的酸酐固化剂一起固化,形成互穿聚合物网络,Tg > 100°C。氨缩水甘油酯衍生物结构中的叔胺基团不仅能加速开环反应,还能充当内部催化剂,激活光聚合物中的游离 -OH 基团和酯分子之间的键交换反应。流变仪研究证实了这一点,该研究显示在温度升高时会出现明显的应力松弛,从而使 3D 打印模具具有可再加工性。利用选定的树脂配方,通过数字光处理三维打印技术打印出一套模具,并成功挤出了高填充度的橡胶复合物。研究结果清楚地表明,具有动态共价键的双固化树脂是一类很有前途的快速模具材料,并为定制和方便地制造橡胶加工挤出模具铺平了道路。本文受版权保护,保留所有权利。
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引用次数: 0
Controlling photopolymerization reaction in layer-by-layer photopolymerization in 3D printing 控制 3D 打印中逐层光聚合反应的光聚合反应
Pub Date : 2024-02-17 DOI: 10.1002/appl.202400004
Xavier Allonas, Ben Hammouda, Boris Métral, Emile Goldbach, Anne-Sophie Schuller, Christian Ley, C.Céline Croutxé-Barghorn

Today, controlling the photopolymerization process during the 3D printing in vat photopolymerization is a key challenge. In this work, it is shown that using a relatively limited set of parameter, it is possible to estimate key factors involved in such process. On the basis of 16 formulations containing different concentrations of photoinitiator and UV filter, attempt was made to rationalize the photonic parameters used in the 3D printing process, that is, the depth of penetration Dp and the critical energy Ec. It is shown that the experimental Dp values can be correlated with calculated ones from Bouguer–Beer–Lambert law. Real-time Fourier-transform infrared spectroscopy (RT-FTIR) experiments were performed under similar conditions as in 3D printing. The conversion profiles were used to estimate the Ec values. The limits of this approach was discussed as a function of the UV filter concentration. Finally, the RT-FTIR curves are exploited to predict the in-depth conversion of the different 3D printed layers and compared to experimental results obtained by confocal Raman microscopy.

如今,在大桶光聚合 3D 打印过程中控制光聚合过程是一项关键挑战。这项研究表明,使用一组相对有限的参数,就有可能估算出此类过程中涉及的关键因素。根据含有不同浓度光引发剂和紫外线过滤器的 16 种配方,尝试对 3D 打印过程中使用的光子参数(即穿透深度 Dp 和临界能量 Ec)进行合理化。实验结果表明,实验得出的 Dp 值与根据布格-比尔-朗伯定律计算得出的 Dp 值具有相关性。实时傅立叶变换红外实验是在与 3D 打印类似的条件下进行的。转换曲线用于估算 Ec 值。讨论了这种方法的局限性与紫外线滤光片浓度的函数关系。最后,利用 RT-FTIR 曲线预测了不同 3D 打印层的深度转换,并与共焦拉曼显微镜获得的实验结果进行了比较。本文受版权保护。
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