DMA

DMA
  • 文章类型: Journal Article
    通过传统方法合成石墨烯具有几个缺点,例如释放有毒气体,这些技术大多耗时且乏味,除了在合成过程中不控制石墨烯的结构组成。在这项研究中,在250°C和270°C的温和环境下,通过壳聚糖的直接溶剂热处理,从新型前体壳聚糖合成氮掺杂的石墨烯(N-掺杂石墨烯(NG))的简便方法。十六烷基三甲基溴化铵(CTAB)和氨被用作结构导向剂。FTIR,XRD,CHNS/O元素分析,XPS,和拉曼光谱用于阐明N-掺杂石墨烯的化学组成和纯度。利用SEM对NG的表面形貌进行了研究,HR-TEM,和选定区域电子衍射(SAED)。结果证明,一罐,单步法是一种简单且经济有效的技术,用于生产高产量的NG,迷人的微观结构特征,包括良好的石墨化,低氧化态,良好的去角质水平,和非常延伸的横向尺寸表。已经提出了关于增长机制的深刻愿景。还研究了NG在水泥砂浆中的掺入效果。两个百分比的NG0.05wt%和,使用总水泥质量的0.10重量%。通过进行AFM研究了水泥砂浆上掺入NG的微观结构研究,和SEM。此外,可加工性和机械特性,包括,抗压强度,和抗弯强度进行了研究。此外,研究了储能模量和损耗因子等动态力学参数。注意到,随着分别添加0.05重量%和0.1重量%的NG,可加工性从14.8%降低至7.8%。然而,对于含有0.1wt%NG的砂浆,抗压强度的最大增量为35%,弯曲强度比未改性的砂浆增加了三倍。此外,与未改性的IMPa相比,含有0.1重量%NG的水泥砂浆具有12MPa的储能模量,并且具有最低的损耗因子(阻尼系数)。这些结果验证了在水泥中掺入NG纳米片对增强水泥砂浆具有积极作用。
    The synthesis of graphene via traditional methods has several drawbacks, such as the release of poisonous gases, Most of these techniques are time-consuming and tedious, besides the absence of control over the structural composition of graphene during synthesis. In this study, a facile approach for the synthesis of graphene densely doped with nitrogen (N-dopped graphene (NG)) from novel precursor chitosan throughout the direct solvothermal treatment of chitosan under mild circumstances at 250 °C and 270 °C. Cetyltrimethylammonium bromide (CTAB) and ammonia are utilized as structural directing agents. FTIR, XRD, CHNS/O elemental analysis, XPS, and Raman spectroscopy are utilized to elucidate the chemical composition and purity of N-dopped graphene. The surface morphology of NG is studied by using SEM, HR-TEM, and selected area electron diffraction (SAED). The results approved that, the one-pot, single-step approach is a simple and cost-effective technique for producing a high throughput of NG, of charming microstructure features, including good graphitization, low oxidation state, good exfoliation level, and very extended lateral dimension sheets. Profound visions on the growing mechanism have been proposed. The incorporation effect of NG to cement mortar is also studied. Two percentages of NG 0.05 wt% and, 0.10 wt% from the total cement mass were utilized. A microstructural investigation of incorporated NG on cement mortar is studied by conducting AFM, and SEM. Furthermore, workability and mechanical characterizations including, compressive strength, and flexural strength are investigated. Also, the dynamic mechanical parameters including storage modulus and loss factor are studied. It is noticed that the workability decreased from 14.8 % to 7.8 % with the addition of 0.05 wt% and 0.1 wt% NG respectively. However, the maximum increments of the compressive strength were 35 % for the mortar containing 0.1 wt% NG and flexural strength increased three times than the unmodified one. Also, the cement mortar containing 0.1 wt% NG has a storage modulus of 12 MPa compared to unmodified 1 MPa and has the lowest loss factor (damping coefficient). These results verified that incorporating NG nanosheets in cement has a positive effect on reinforcing cement mortar.
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  • 文章类型: Journal Article
    这项研究描述了一种新的生物基环氧树脂热固性材料的生产及其与长麻纤维一起使用,以生产完全基于生物的高性能复合材料。BioIgenox的合成,来自木质素生物炼制的环氧树脂,其固化过程已经过优化,以减少其对环境的影响。这项研究的主要目的是表征环氧树脂体系的流变性和动力学,以优化复合材料的制造过程。因此,环氧树脂/硬化剂系统的选择是考虑到植物纤维增强复合材料的实施所施加的限制。所选混合物的粘度表明配方与复合材料的传统实施方法的相容性。此外,与BPA-双酚A(DGEBA)环氧树脂的二缩水甘油醚的前体不同,BioIgenox及其前体没有内分泌干扰活性。使用三点弯曲测试表征纯聚合物及其单向大麻纤维复合材料。对完全生物基环氧聚合物的测量结果显示弯曲模量,弯曲强度,破坏时的最大应变和Tg为,分别,3.1GPa,55MPa,1.82%和120℃这些值比基于DGEBA的环氧材料的值稍弱。还观察到,将纤维结合到完全生物基环氧体系中引起阻尼峰的降低和向更高温度的偏移。这些结果指出了大麻纤维和完全生物基环氧树脂体系之间的有效应力传递。在这项工作中使用完全生物基环氧体系测量的高机械性能和软化温度使这种复合材料成为运输和轻质工程应用的非常有前途的可持续材料。
    This study describes the production of a new biobased epoxy thermoset and its use with long hemp fibres to produce high-performance composites that are totally biobased. The synthesis of BioIgenox, an epoxy resin derived from a lignin biorefinery, and its curing process have been optimised to decrease their environmental impact. The main objective of this study is to characterise the rheology and kinetics of the epoxy system with a view to optimising the composite manufacturing process. Thus, the epoxy resin/hardener system was chosen considering the constraints imposed by the implementation of composites reinforced with plant fibres. The viscosity of the chosen mixture shows the compatibility of the formulation with the traditional implementation processes of the composites. In addition, unlike BPA-a precursor of diglycidyl ether of bisphenol A (DGEBA) epoxy resin-BioIgenox and its precursor do not have endocrine disrupting activities. The neat polymer and its unidirectional hemp fibre composite are characterised using three-point bending tests. Results measured for the fully biobased epoxy polymer show a bending modulus, a bending strength, a maximum strain at failure and a Tg of, respectively, 3.1 GPa, 55 MPa, 1.82% and 120 °C. These values are slightly weaker than those of the DGEBA-based epoxy material. It was also observed that the incorporation of fibres into the fully biobased epoxy system induces a decrease in the damping peak and a shift towards higher temperatures. These results point out the effective stress transfers between the hemp fibres and the fully biobased epoxy system. The high mechanical properties and softening temperature measured in this work with a fully biobased epoxy system make this type of composite a very promising sustainable material for transport and lightweight engineering applications.
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  • 文章类型: Journal Article
    水凝胶已被广泛研究用于生物医学应用,如药物递送,组织工程支架,和生物传感器。尽管需要这种类型的经验数据来推进创新的生物医学设计的设计并为数值模型提供信息,但文献中关于经受高应变动态载荷条件的水凝胶材料的机械性能存在差距。对于这项工作,使用光聚合方法制造HEMA-DMAEMA水凝胶。水凝胶以等于50%的应变率承受高压缩振荡动态机械载荷,60%,70%,随着时间的推移,观察到储存和损耗模量,例如,72h和5、10和15天。不出所料,增加的菌株导致较低的储存和损耗模量,这可能归因于水凝胶网络的破坏,例如,网络中断增加,链条断裂或打滑,和部分塑性变形。这项研究有助于促进我们对承受高应变率的水凝胶的理解,以了解其粘弹性行为,即,应变率灵敏度,能量耗散机制,和变形动力学,在实际应用中,需要对水凝胶行为进行精确建模和预测。
    Hydrogels have been extensively studied for biomedical applications such as drug delivery, tissue-engineered scaffolds, and biosensors. There is a gap in the literature pertaining to the mechanical properties of hydrogel materials subjected to high-strain dynamic-loading conditions even though empirical data of this type are needed to advance the design of innovative biomedical designs and inform numerical models. For this work, HEMA-DMAEMA hydrogels are fabricated using a photopolymerization approach. Hydrogels are subjected to high-compression oscillatory dynamic mechanical loading at strain rates equal to 50%, 60%, and 70%, and storage and loss moduli are observed over time, e.g., 72 h and 5, 10, and 15 days. As expected, the increased strains resulted in lower storage and loss moduli, which could be attributed to a breakdown in the hydrogel network attributed to several mechanisms, e.g., increased network disruption, chain scission or slippage, and partial plastic deformation. This study helps to advance our understanding of hydrogels subjected to high strain rates to understand their viscoelastic behavior, i.e., strain rate sensitivity, energy dissipation mechanisms, and deformation kinetics, which are needed for the accurate modeling and prediction of hydrogel behavior in real-world applications.
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  • 文章类型: Journal Article
    官能化咪唑并[1,2-α]吡啶是药物中重要的支架。在这里,我们通过FeCl3催化的三组分偶联反应,在DMA和H2O(2:1)中通过亚硫酸钠为咪唑并[1,2-α]吡啶提供了有效的3-磺酰基甲基化方案。因此,以高产率提供了各种磺酰基甲基咪唑并[1,2-α]吡啶,并具有出色的官能团耐受性。提出了一种合理的氧化加成机理。
    Functionalized imidazo[1,2-α]pyridines are important scaffolds in pharmaceuticals. Herein, we present an efficient 3-sulfonylmethylation protocol for imidazo[1,2-α]pyridines by sodium sulfinates in DMA and H2O (2:1) via an FeCl3-catalyzed three-component coupling reaction. Various sulfonylmethyl imidazo[1,2-α]pyridines were thus afforded in high yields with excellent functional group tolerance. A plausible oxidation-addition mechanism was proposed.
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  • 文章类型: Journal Article
    在目前的研究中,尝试通过生物启发化学方法合成羟基磷灰石-二氧化铈(HAP-CeO2)支架。所用的胶体CeO2悬浮液在浓度高于86.1ppm时对黄曲霉和烟曲霉具有抗真菌活性。生产了三种不同系列的复合HAP-CeO2悬浮液,基于向其中加入CeO2悬浮液的前体悬浮液和通过该加入是在羟基磷灰石相形成之前还是之后进行区分。每个系列由三个悬架组成,其中纯二氧化铈重量达到所产生的羟基磷灰石的4、5和10%(按质量计),分别。表征表明,2S系列的标本对其粘弹性能表现出更大的变化。此外,具有4%CeO2的2S系列样品表现出最佳的机械响应。这是由于冻干过程中针状HAP晶体的生长,当垂直于应力施加方向取向时,可以增强样品的抗变形能力。2S系列支架的平均孔径等于100μm,最小开孔率为89.5%,同时在磷酸盐缓冲盐水中的溶解速率最低。
    In the current study, the synthesis of hydroxyapatite-ceria (HAP-CeO2) scaffolds is attempted through a bioinspired chemical approach. The utilized colloidal CeO2 suspension presents antifungal activity against the Aspergillus flavus and Aspergillus fumigatus species at concentrations higher than 86.1 ppm. Three different series of the composite HAP-CeO2 suspensions are produced, which are differentiated based on the precursor suspension to which the CeO2 suspension is added and by whether this addition takes place before or after the formation of the hydroxyapatite phase. Each of the series consists of three suspensions, in which the pure ceria weight reaches 4, 5, and 10% (by mass) of the produced hydroxyapatite, respectively. The characterization showed that the 2S series\'s specimens present the greater alteration towards their viscoelastic properties. Furthermore, the 2S series\'s sample with 4% CeO2 presents the best mechanical response. This is due to the growth of needle-like HAP crystals during lyophilization, which-when oriented perpendicular to the direction of stress application-enhance the resistance of the sample to deformation. The 2S series\'s scaffolds had an average pore size equal to 100 μm and minimum open porosity 89.5% while simultaneously presented the lowest dissolution rate in phosphate buffered saline.
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  • 文章类型: Journal Article
    鉴于探索航空航天废料升级的可能性,本研究研究了不合格碳纤维预浸料的固化特性。使用动态机械分析仪(DMA)以材料的机械固化转化状态的形式检查预浸料的固化行为。通过比较反应开始时的储能模量(E'0)和等温实验期间的瞬时储能模量(E't)与从动态扫描获得的完全固化材料的储能模量(E'∞),对固化动力学进行建模。使用DiBenedetto模型对玻璃化转变温度Tg和凝胶化之前的反应程度进行建模,其中每个层压板的Tg在DMA中确定,根据标准ASTMD7028。机械性能,治愈的程度,根据工业和国际标准确定固化层压材料的玻璃化转变温度。在100°C和140°C之间的温度下的最大转化率为约80%(±5%)。模型的转换率与实验数据显示出合理的匹配,在约30-40%的固化转化率下表现出最大反应速率。使用DiBenedetto模型的作为固化转化函数的Tg的预测演变提供了与实验数据的94%匹配。基于模型的多级固化周期提供更短的周期时间和高质量的层压板。机械测试结果表明,拉伸强度和模量降低了约13%和15%,分别,与原始的相比。固化层压材料的固化实验程度(95.4%)与模型预测的程度(97%)非常一致。层压板的孔隙率估计约为2.4%,这在一些行业中是可以接受的。
    In view of exploring the possibility of upcycling aerospace scrap, cure characteristics of out-of-spec carbon fiber prepregs are investigated in this study. The cure behavior of the prepreg is examined in the form of the mechanical cure conversion state of the material using a Dynamic Mechanical Analyzer (DMA). Cure kinetics is modeled by comparing the storage modulus at the start of the reaction (E\'0) and instantaneously (E\'t) during isothermal experiments with those of the fully cured material (E\'∞) obtained from dynamic scans. The glass transition temperature Tg and the extent of reaction before gelation are modeled using the DiBenedetto model, where the Tg of each laminate is determined in a DMA, per standard ASTM D7028. The mechanical properties, the extent of cure, and the glass transition temperature of the cured laminates were determined according to industry and international standards. The maximum conversion at temperatures between 100 °C and 140 °C is approximately 80% (±5%). The modeled rate of conversion shows a reasonable match with the experimental data, exhibiting a maximum reaction rate at about 30-40% of the cure conversion. The predicted evolution of the Tg as a function of cure conversion using the DiBenedetto model provides a 94% match with the experimental data. The multi-stage cure cycle based on the models offers shorter cycle times and high-quality laminates. The mechanical test results indicate approximately a 13% and 15% decrease in tensile strength and modulus, respectively, compared to pristine ones. The experimental extent of cure of the cured laminates (95.4%) is in close agreement with that predicted by the model (97%). The porosity in the laminates is estimated to be approximately 2.4%, which is acceptable in several industries.
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  • 文章类型: Journal Article
    不断增加的废橡胶回收利用为许多有价值的应用产生了一系列似是而非的产品。制备了不同浓度的废橡胶/三元乙丙橡胶复合材料。红外光谱(FTIR)用于鉴定化学成分。吸水性试验,动态力学分析(DMA),进行和热重分析(TGA)。(75/25)WR/EPDM橡胶复合材料表现出最佳的性能和最高的机械性能。将Fe2O3添加到(75/25)WR/EPDM橡胶复合材料中。吸水率,FTIR,TGA,和DMA进行了调查。随着Fe2O3含量的增加,复合性能得到改善。还使用137Cs点源测量了线性衰减系数(μ),该系数是γ射线能量662keV的Fe2O3浓度的函数;辐射屏蔽可以用参数的数量来表示,例如质量衰减系数(μm),半值层(HVL),第十值层TVL和辐射防护效率(RPE%),辐射防护效率随着Fe2O3的增加而增加。
    Increasing waste rubber recycling produces a specious range of products for many valuable applications. Waste Rubber/EPDM composite with different concentrations was prepared. Infrared spectroscopy (FTIR) is used to identify the chemical composition. A water absorption test, Dynamic mechanical analysis (DMA), and Thermal Gravimetric Analysis (TGA) were performed. The (75/25) WR/EPDM rubber composite exhibited the best behavior with the highest mechanical performance. Fe2O3 was added to (75/25) WR/EPDM rubber composite. Water absorption, FTIR, TGA, and DMA were investigated. The composite performance was improved with increasing Fe2O3 content. The linear attenuation coefficients (μ) were also measured as a function of the concentrations of Fe2O3 for γ-ray energy 662 keV by using 137Cs point source; the radiation shielding can be denoted by numbers of parameters like mass attenuation coefficient (μm), half value layer (HVL), Tenth value layer TVL and radiation protection efficiency (RPE%), radiation protection efficiency increased as Fe2O3 increased.
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  • 文章类型: Journal Article
    人类体内的汞毒性很高,因此有必要监测食品中的汞含量,制药,和环境,以尽量减少人类暴露。在2020年6月至2021年10月期间,研究人员从也门海岸的不同地点收集了240个鱼类样本,以评估汞污染情况。使用直接汞分析仪测定每个样品中的汞浓度。为了确保方法的准确性,进行了一系列一式三份的汞浓度分析。样品范围从2到100纳克,以确定线性和重复性,即,日内变化。结果显示了很高的精确度,相关系数为0.9990,重复性为1.34%-5.62%。该方法准确度高,因为受污染的鱼类样品的汞回收率从96.77%到105.14%不等。汞的检测限和定量限分别为0.0015ppm和0.0049ppm,分别。这使得该方法能够检测鱼肉中的痕量汞。240个鱼类样本中的汞浓度没有超过FDA,但低于YSMO规定的0.5ppm限值。
    The high levels of mercury toxicity in humans make it necessary to monitor mercury levels in food, pharmaceuticals, and the environment to minimize human exposure. Between June 2020 and October 2021, researchers collected 240 fish samples from different locations along the Yemeni coast to evaluate mercury contamination. The Direct Mercury Analyzer was used to determine the concentration of mercury in each sample. To ensure method accuracy, a series of triplicate mercury concentration analyses were conducted. The samples ranged from 2 to 100 ng to determine linearity and repeatability i.e., within-day variation. The results showed a high level of precision, with a correlation coefficient of 0.9990 and a repeatability of 1.34 %-5.62 % RSD range. The method was also highly accurate, as the mercury recovery results from the contaminated fish samples ranged from 96.77 % to 105.14 %. The limits of detection and quantitation of mercury were 0.0015 ppm and 0.0049 ppm, respectively. This allowed the method to detect trace amounts of mercury in fish meat. Mercury concentration in the 240 fish samples did not exceed the FDA, but below the 0.5 ppm specified limit of YSMO.
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  • 文章类型: Journal Article
    聚合物共混物用于生产用于增材制造的长丝以平衡机械和加工性能。由聚乳酸(PLA)制成的聚合物长丝的机械和热性能,聚羟基链烷酸酯(PHA),本文研究了其共混物(PLA-PHA),并将其与测得的结构和物理化学性质相关联。PLA具有最高的刚度和抗拉强度,但韧性较低。PLA-PHA共混物的力学性能与PLA相似,但具有明显更高的韧性。尽管纯PHA的机械性能较低,掺入少量(12重量%。%)的PHA与纯PLA相比显著提高了韧性(约50%)。协同效应归因于PLA中混合PHA的球晶形态,促进两种聚合物的无定形区域之间的相互作用。PLA-PHA共混物的热稳定性显著提高,通过热重分析确定。与PLA相比,共混物还表现出较低的冷结晶和玻璃化转变温度,这有利于增材制造。在增材制造之后,X射线光电子能谱表明,三根细丝的C-C和C=O键增加,与C-O键的损失有关。由于链重组,热过程引起PHA结晶度的轻微增加。该研究提供了对增材制造熔化过程中发生的热和结构变化的见解。
    Polymeric blends are employed in the production of filaments for additive manufacturing to balance mechanical and processability properties. The mechanical and thermal properties of polymeric filaments made of poly (lactic acid) (PLA), polyhydroxyalkanoates (PHA), and its blend (PLA-PHA) are investigated herein and correlated to their measured structural and physicochemical properties. PLA exhibits the highest stiffness and tensile strength, but lower toughness. The mechanical properties of the PLA-PHA blend were similar to those of PLA, but with a significantly higher toughness. Despite the lower mechanical properties of neat PHA, incorporating a small amount (12 wt.%) of PHA into PLA significantly enhances toughness (approximately 50%) compared to pure PLA. The synergistic effect is attributed to the spherulitic morphology of blended PHA in PLA, promoting interactions between the amorphous regions of both polymers. Thermal stability is notably improved in the PLA-PHA blend, as determined by thermogravimetric analysis. The blend also exhibits lower cold crystallization and glass transition temperatures as compared to PLA, which is beneficial for additive manufacturing. Following additive manufacturing, X-ray photoelectron spectroscopic showed that the three filaments present an increase in C-C and C=O bonds associated with the loss of C-O bonds. The thermal process induces a slight increase in crystallinity in PHA due to chain reorganization. The study provides insights into the thermal and structural changes occurring during the melting process of additive manufacturing.
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  • 文章类型: Journal Article
    未来粒子加速器的超导磁体将在低温下暴露于高辐照剂量。为了研究辐照温度和气氛对老化行为的影响,我们已经表征了六种环氧树脂的热机械性能的变化,这些环氧树脂在环境空气中辐照高达20MGy后,可能用于超导磁体。惰性气体,和液氦.根据动态力学分析(DMA)的结果,我们讨论了辐照温度和氧气存在的影响。辐照温度对交联和断链发生的速率有很大影响。
    The superconducting magnets of future particle accelerators will be exposed to high irradiation doses at cryogenic temperatures. To investigate the effect of irradiation temperature and atmosphere on the aging behavior, we have characterized the changes in thermomechanical properties of six epoxy resins for potential use in superconducting magnets after irradiation up to 20 MGy in ambient air, inert gas, and liquid helium. Based on the results obtained by Dynamic Mechanical Analysis (DMA), we discuss the effect of irradiation temperature and the presence of oxygen. The irradiation temperature can have a strong influence on the rates at which cross-linking and chain scission occur.
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