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Effectiveness of a silane coupling agent in a resin luting cement 树脂胶合剂中硅烷偶联剂的功效
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-14 DOI: 10.1016/j.ijadhadh.2024.103808

The objective of this study was to investigate a new silane-containing self-adhesive resin luting cement with both shear bond strength and contact angle studies to determine if silane in a resin cement would chemically bond to a lithium disilicate surface. The silane-containing cement, Panavia SA Cement Universal (Kuraray, Tokyo, Japan) was tested against a control case where a traditional silane treatment was paired with resin-luting cement, Duo-Link Universal (Bisco Inc., Schaumburg, IL, USA) with immediate shear bond strength testing on both polished and etched lithium disilicate, as well as after thermocycling. It was determined that micromechanical retention provided a substantial contribution to bond strength. However, after an aging study with 20,000 thermocycles and then storage for 6 months in 37 °C water, the silane-containing, self-adhesive resin cement significantly decreased in shear bond strength when compared to the control. From contact angle studies, while it was shown that the paste containing the silane did effectively increase hydrophobicity of the treated lithium disilicate surface, it required over 3 h contact time, which was not representative of clinical use.

本研究的目的是通过剪切粘结强度和接触角研究来确定树脂粘结剂中的硅烷是否会与二硅酸锂表面发生化学粘结,从而研究一种新型含硅烷的自粘树脂粘结剂。我们将含硅烷的水泥 Panavia SA Cement Universal(可乐丽,日本东京)与传统硅烷处理的树脂衬垫水泥 Duo-Link Universal(Bisco Inc.结果表明,微机械保留对粘接强度有很大的贡献。然而,在经过 20,000 次热循环和在 37 °C 水中存放 6 个月的老化研究后,与对照组相比,含硅烷的自粘性树脂粘接剂的剪切粘接强度明显下降。接触角研究表明,虽然含有硅烷的浆料确实有效地增加了经处理的二硅酸锂表面的疏水性,但它需要超过 3 小时的接触时间,这在临床使用中并不具有代表性。
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引用次数: 0
Evaluation of the optimal etching times and fissure sealant materials for bonding on primary teeth enamel: An in vitro study 评估用于粘接乳牙釉质的最佳蚀刻时间和窝沟封闭材料:体外研究
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-13 DOI: 10.1016/j.ijadhadh.2024.103811

The recommended 15-s acid etching time expands the enamel surface and facilitates the infiltration of restorative materials. Because of this clinical advantage, 15 and 30 s have become the most prevalent acid etching times in recent years. This study aimed to evaluate the effects of conventional and self-adhesive flowable composites (SAFCs) that were etched for different durations on primary molar teeth. Teeth were divided into eight groups (n = 16) and restored either with Vertise™ Flow and orthophosphoric acid or with Conseal F and orthophosphoric acid for 15, 30, 45, or 60 s. Then, the specimens were subjected to shear stress at a cross-head speed of 1 mm/min until the bond failed. After conducting the microshear bond strength (μSBS) test, failure modes were analyzed using scanning electron microscopy at 80 × magnification. Statistical analysis was performed using Independent sample T-tests and other T-tests (p < 0.05). According to the μSBS results, a statistically significant difference was observed among all groups (p < 0.05). Additionally, there were statistically significant differences between both restorative materials after etching for 15 s (p = 0.011; p < 0.05) and 60 s (p < 0.001; p < 0.05). While adhesive-type fractures were mostly observed in the SAFC groups, mixed-type fractures analyzed by scanning electron microscopy were determined to be relatively common in the Conseal F groups. An etching time of 15 s for primary tooth enamel was recommended instead of 60 s for all fissure sealants. In addition, the application of Vertise™ Flow after 15 s of acid etching was preferred over the application of Conseal F.

建议的 15 秒酸蚀时间可以扩展釉质表面,有利于修复材料的渗入。由于这种临床优势,15 秒和 30 秒已成为近年来最常用的酸蚀时间。本研究旨在评估传统和自粘性可流动复合材料(SAFCs)不同酸蚀时间对初级磨牙的影响。将牙齿分为八组(n = 16),分别用 Vertise™ Flow 和正磷酸或 Conseal F 和正磷酸修复 15、30、45 或 60 秒。然后,以 1 mm/min 的十字头速度对试样施加剪切应力,直至粘接失败。在进行微剪切粘接强度(μSBS)测试后,使用放大 80 倍的扫描电子显微镜分析失效模式。统计分析采用独立样本 T 检验和其他 T 检验(p < 0.05)。根据 μSBS 结果,各组之间的差异具有统计学意义(p < 0.05)。此外,两种修复材料在蚀刻 15 秒(p = 0.011;p <;0.05)和 60 秒(p <;0.001;p <;0.05)后的差异也有统计学意义。通过扫描电子显微镜分析发现,粘合型断裂主要出现在 SAFC 组中,而混合型断裂在 Conseal F 组中相对常见。建议对原生牙釉质的蚀刻时间为 15 秒,而不是所有裂隙封闭剂的 60 秒。此外,酸蚀 15 秒后使用 Vertise™ Flow 比使用 Conseal F 更可取。
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引用次数: 0
Imparting semi-permanent demoldability to stainless steel mold using surface-initiated solution polymerization of stearyl methacrylate 利用甲基丙烯酸硬脂酯的表面引发溶液聚合使不锈钢模具具有半永久脱模性
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-13 DOI: 10.1016/j.ijadhadh.2024.103812

The growing market demand for compact and precisely-designed polymeric products has raised challenges during the demolding stage of manufacturing. An increased contact area between the product and the mold increases adhesion, which reduces dimensional stability and aesthetics. Conventional solutions like surface roughness improvement or release agent coatings suffer from reduced productivity and impurity-related issues affecting mechanical properties. To address these challenges, we imparted the semi-permanent demoldability to a stainless steel (SUS) mold by polymerizing stearyl methacrylate monomer on its surface using a surface-initiated solution polymerization technique. The polymerization state was confirmed through Fourier transform infrared spectroscopy and field emission scanning electron microscopy. The demoldablity was investigated using the appropriately-designed lap shear tests to simulate the demolding stage of epoxy resin-filled SUS mold to ensure sufficient performance compared with the neat and commercial release agent (RA) treated molds, and durability of the demoldability was confirmed via repetitive single-lap shear tests simulating the molding and demolding processes. The surfaced polymerized mold exhibited excellent demoldability with 96.5 % improvement over the neat one, and showed excellent durability over 5 repeated molding cycles, while the commercial RA showed significant degradation of demoldability. Furthermore, the mechanism of demoldability enhancement using the proposed surface polymerization was investigated by characterization of the surface dewetting pattern and contact angle measurements of the epoxy resin on the modified mold surface.

市场对结构紧凑、设计精确的聚合物产品的需求日益增长,这给生产过程中的脱模阶段带来了挑战。产品与模具之间的接触面积增大会增加附着力,从而降低尺寸稳定性和美观度。传统的解决方案,如改善表面粗糙度或脱模剂涂层等,都会降低生产率,并产生与杂质相关的问题,影响机械性能。为了应对这些挑战,我们采用表面引发的溶液聚合技术,在不锈钢(SUS)模具表面聚合甲基丙烯酸硬脂酯单体,赋予其半永久脱模性。聚合状态通过傅立叶变换红外光谱和场发射扫描电子显微镜进行了确认。通过适当设计的搭接剪切试验来模拟环氧树脂填充 SUS 模具的脱模阶段,以考察其脱模性,从而确保与未添加脱模剂(RA)的模具和经脱模剂(RA)处理的模具相比,具有足够的脱模性能,并通过模拟成型和脱模过程的重复单搭接剪切试验来确认脱模性的持久性。经过表面聚合处理的模具表现出极佳的脱模性,与未经过表面聚合处理的模具相比,脱模性提高了 96.5%,并且在重复 5 次成型循环后表现出极佳的耐久性,而经过商业脱模剂处理的模具则表现出明显的脱模性下降。此外,还通过对改性模具表面的环氧树脂露湿模式和接触角测量结果进行表征,研究了利用拟议的表面聚合提高脱模性的机理。
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引用次数: 0
Study on the influence of FCC waste catalysts on the interaction ability between asphalt and fillers 催化裂化废催化剂对沥青与填料相互作用能力的影响研究
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-10 DOI: 10.1016/j.ijadhadh.2024.103810

Fluid catalytic cracking (FCC) waste catalysts produced by petroleum cracking contain many harmful substances, such as heavy metals, and improper treatment can lead to environmental pollution. To solve this problem, this study investigated four types of FCC (LM, SH, A, SL) waste catalyst as a substitute filler for limestone mineral powder and examined their interactions with asphalt and fillers. The X-ray fluorescence (XRF), scanning electron microscope and specific surface area tests were conducted to compare the performance of FCC waste catalyst and fillers. Meanwhile, the effects of FCC waste catalyst on asphalt mastic composed of limestone mineral powder and asphalt were evaluated using surface energy, interaction parameters, and FTIR. Results show that there is little difference in the main components of the four waste FCC catalysts and limestone mineral powder. However, the surface roughness and specific surface area of the FCC catalysts are significantly greater than those of limestone. Moreover, the addition of FCC waste catalyst can improve the adhesion of asphalt with fillers and aggregates, and significantly enhance the interaction capabilities between the filler and the base asphalt, especially for SH. FTIR analysis confirms that the aforementioned improvements are achieved through physical interactions. This study reveals the effects of different FCC waste catalysts on asphalt mortar, and provides a theoretical basis for promoting the practical application of FCC waste catalysts in road engineering.

石油裂解产生的流体催化裂化(FCC)废催化剂含有重金属等多种有害物质,处理不当会造成环境污染。为解决这一问题,本研究将四种催化裂化废催化剂(LM、SH、A、SL)作为石灰石矿粉的替代填料,并考察了它们与沥青和填料的相互作用。通过 X 射线荧光 (XRF)、扫描电子显微镜和比表面积测试来比较催化裂化废催化剂和填料的性能。同时,利用表面能、相互作用参数和傅立叶变换红外光谱评估了催化裂化废催化剂对由石灰石矿粉和沥青组成的沥青胶泥的影响。结果表明,四种催化裂化废催化剂和石灰石矿粉的主要成分差别不大。但是,催化裂化催化剂的表面粗糙度和比表面积明显大于石灰石。此外,添加催化裂化废催化剂可改善沥青与填料和集料的粘附性,显著增强填料与基质沥青之间的相互作用能力,尤其是对 SH 而言。傅立叶变换红外分析证实,上述改善是通过物理相互作用实现的。本研究揭示了不同催化裂化废催化剂对沥青砂浆的影响,为促进催化裂化废催化剂在道路工程中的实际应用提供了理论依据。
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引用次数: 0
Evaluation of the shear bond strength between CAD/CAM blocks and sonic/thermoviscous bulk-fill composites with different surface treatments 评估不同表面处理的 CAD/CAM 块与声波/热粘散装填充复合材料之间的剪切粘接强度
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-09 DOI: 10.1016/j.ijadhadh.2024.103805

Background/purpose

To evaluate the shear bond strength (SBS) of nanoceramic hybrid CAD/CAM blocks with two bulk-fill composites in deep margin elevation following different surface pretreatments.

Materials and methods

Forty cylindrical-shaped samples (3 mm diameter × 4 mm height) were prepared from each group of bulk-fill resin composites (BRC) (SonicFill 3/SF, VisCalor bulk/VS), and 80 samples (14.5 mm × 7.2 mm × 2 mm) were sectioned from Grandio Block. Specimens of each BRC were assigned to two subgroups, and surfaces of one group were treated with a tribochemical silica-coating. The CAD/CAM block sample surfaces were treated with Al2O3 particles. CAD/CAM block and composite samples were luted using dual-cure universal resin-based cement (Bifix QM). Following immersion in distilled water for 24 h, the samples were divided as immediate and test groups. The test group was subjected to thermocycle (5–55 °C, 10,000 cycles). The SBS of the resin-based cement between the blocks and BRC was tested on a universal testing device until failure. Failure type was determined using a stereomicroscope. The roughening pattern was evaluated with SEM. Statistical analysis included Shapiro Wilk, Generalized Linear Models, and Fisher's Exact tests (P < 0.05).

Results

No statistically significant difference was found between the mean SBS values according to deep margin elevation materials and surface pretreatment (P > 0.05). Aging procedure resulted in a statistically significant difference between the mean SBS values (P < 0.001). While the mean SBS value was 33.7 ± 7.9 MPa in immediate group, it was calculated as 22.6 ± 6.3 MPa in test group following thermocycle.

Conclusion

In terms of SBS, both bulk-fill resin composites performed similarly. Although higher SBS values were obtained with tribochemical silica-coating, the adverse effects of thermocycling on bonding could not be prevented.

评估纳米陶瓷混合 CAD/CAM 块体与两种大量填充复合材料在不同表面预处理后的深边缘隆起剪切粘接强度(SBS)。从每组团状填充树脂复合材料(BRC)(SonicFill 3/SF、VisCalor bulk/VS)中制备 40 个圆柱形样品(直径 3 毫米×高 4 毫米),从 Grandio Block 中切分 80 个样品(14.5 毫米×7.2 毫米×2 毫米)。每个 BRC 样品被分成两组,其中一组的表面经过摩擦化学二氧化硅涂层处理。CAD/CAM 块样本表面用氧化铝颗粒处理。使用双固化通用树脂基水泥(Bifix QM)对 CAD/CAM 块和复合材料样品进行砌筑。在蒸馏水中浸泡 24 小时后,样品被分为直接组和测试组。测试组进行热循环(5-55 °C,10,000 次循环)。砌块和 BRC 之间树脂基水泥的 SBS 在通用测试装置上进行测试,直至失效。使用体视显微镜确定失效类型。用扫描电子显微镜对粗糙模式进行评估。统计分析包括 Shapiro Wilk 检验、广义线性模型检验和费雪精确检验(0.05)。老化过程导致平均 SBS 值之间存在显著的统计学差异 ( < 0.001)。即时组的平均 SBS 值为 33.7 ± 7.9 兆帕,而热循环后测试组的平均 SBS 值为 22.6 ± 6.3 兆帕。就 SBS 值而言,两种填充树脂复合材料的表现相似。虽然摩擦化学二氧化硅涂层获得了更高的 SBS 值,但热循环对粘合的不利影响无法避免。
{"title":"Evaluation of the shear bond strength between CAD/CAM blocks and sonic/thermoviscous bulk-fill composites with different surface treatments","authors":"","doi":"10.1016/j.ijadhadh.2024.103805","DOIUrl":"10.1016/j.ijadhadh.2024.103805","url":null,"abstract":"<div><h3>Background/purpose</h3><p>To evaluate the shear bond strength (SBS) of nanoceramic hybrid CAD/CAM blocks with two bulk-fill composites in deep margin elevation following different surface pretreatments.</p></div><div><h3>Materials and methods</h3><p>Forty cylindrical-shaped samples (3 mm diameter × 4 mm height) were prepared from each group of bulk-fill resin composites (BRC) (SonicFill 3/SF, VisCalor bulk/VS), and 80 samples (14.5 mm × 7.2 mm × 2 mm) were sectioned from Grandio Block. Specimens of each BRC were assigned to two subgroups, and surfaces of one group were treated with a tribochemical silica-coating. The CAD/CAM block sample surfaces were treated with Al<sub>2</sub>O<sub>3</sub> particles. CAD/CAM block and composite samples were luted using dual-cure universal resin-based cement (Bifix QM). Following immersion in distilled water for 24 h, the samples were divided as immediate and test groups. The test group was subjected to thermocycle (5–55 °C, 10,000 cycles). The SBS of the resin-based cement between the blocks and BRC was tested on a universal testing device until failure. Failure type was determined using a stereomicroscope. The roughening pattern was evaluated with SEM. Statistical analysis included Shapiro Wilk, Generalized Linear Models, and Fisher's Exact tests (<em>P</em> &lt; 0.05).</p></div><div><h3>Results</h3><p>No statistically significant difference was found between the mean SBS values according to deep margin elevation materials and surface pretreatment (<em>P</em> &gt; 0.05). Aging procedure resulted in a statistically significant difference between the mean SBS values (<em>P</em> &lt; 0.001). While the mean SBS value was 33.7 ± 7.9 MPa in immediate group, it was calculated as 22.6 ± 6.3 MPa in test group following thermocycle.</p></div><div><h3>Conclusion</h3><p>In terms of SBS, both bulk-fill resin composites performed similarly. Although higher SBS values were obtained with tribochemical silica-coating, the adverse effects of thermocycling on bonding could not be prevented.</p></div>","PeriodicalId":13732,"journal":{"name":"International Journal of Adhesion and Adhesives","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2024-08-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141944276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Study on the shear failure mechanism of vulcanized rubber-metal bonding interface based on cohesive zone model 基于内聚区模型的硫化橡胶-金属粘接界面剪切破坏机理研究
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-08-08 DOI: 10.1016/j.ijadhadh.2024.103807

Rubber-metal bonding interface prone to adhesive failure. Cohesive zone model (CZM) is widely used in numerical simulation analysis of fracture of interfacial mechanics. In this paper, the traction-separation curve of the bonding surface of vulcanized rubber-metal specimen was obtained by tensile shear test and dumbbell rubber uniaxial tensile test. Then, the influence of shear strain of rubber itself was removed by numerical simulation of tensile shear of rubber, so as to identify the CZM parameters of rubber-metal interface.On this basis, a numerical model of the cohesive force of vulcanized rubber-metal was established, and the stress distribution, variation and damage evolution of the interface along the shear direction were analyzed microscopically. The initiation and propagation of cracks are explained and compared with the failure process and phenomenon of the test interface. The traction-displacement relationship curve was analyzed macroscopically, which was consistent with the traction-displacement relationship curve obtained by the experiment, and the error is less than 5 %. The CZM could accurately express the interface mechanical relationship of the experimental specimen. In addition, the influence of the width and length of the bonding interface on the mechanical properties of the bonding is also analyzed. With the increase of the width or length of the bonding interface, the maximum traction force increases linearly, but the relative displacement value of the initial bonding failure remains unchanged, and the length of the bonding interface has a more significant effect on the maximum traction force. The results show that the cohesive zone model can accurately and effectively analyze the shear failure of the vulcanized rubber-metal bonding surface, which provides a reference for the study of the failure of the bonding surface of other elastic composites.

橡胶-金属粘接界面易发生粘接破坏。粘合区模型(CZM)被广泛应用于界面力学断裂的数值模拟分析。本文通过拉伸剪切试验和哑铃橡胶单轴拉伸试验获得了硫化橡胶-金属试样粘接面的牵引-分离曲线。在此基础上,建立了硫化橡胶-金属内聚力数值模型,并对界面沿剪切方向的应力分布、变化及损伤演化进行了微观分析。解释了裂纹的产生和扩展,并与试验界面的破坏过程和现象进行了比较。宏观分析了牵引力-位移关系曲线,与实验得到的牵引力-位移关系曲线一致,误差小于 5%。CZM 可以准确表达实验试样的界面力学关系。此外,还分析了粘接界面的宽度和长度对粘接力学性能的影响。随着粘接界面宽度或长度的增加,最大牵引力呈线性增加,但初始粘接破坏的相对位移值保持不变,粘接界面长度对最大牵引力的影响更为显著。结果表明,内聚区模型能准确有效地分析硫化橡胶-金属粘接面的剪切破坏,为研究其他弹性复合材料粘接面的破坏提供了参考。
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引用次数: 0
Effect of inositol hexaphosphate acid versus polyacrylic acid on dentin properties and adhesion of a self-adhesive restorative material to dentin 六磷酸肌醇与聚丙烯酸对牙本质特性以及自粘性修复材料与牙本质粘附性的影响
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-07-31 DOI: 10.1016/j.ijadhadh.2024.103804

Objective

This study evaluated the effect of 2% inositol hexaphosphate (IP6) and 10% polyacrylic acid (PAA) on dentin surface micromorphology, matrix/mineral ratio, microhardness, and resin−dentin shear bond strength (SBS) of a self-adhesive restorative material (Surefil™ One; Dentsply Sirona, Konstanz, Germany).

Materials and methods

Human permanent molar mid-coronal dentin discs were either not treated (control), conditioned with 10% PAA (Dentin Conditioner, GC, Tokyo, Japan) for 20 s, or etched with 2% IP6 for 20 s. Dentin surface micromorphology (etching pattern), matrix/mineral ratio, and microhardness were characterized by a scanning electron microscope (SEM), a confocal Raman microscope and a microhardness tester using the Vickers indenter, respectively. Sound molars were cut flat, mounted, surface treated and restored with Surefil™ One, Dentsply. The shear bond strength (SBS) was evaluated using a universal testing machine at 24 h and after 10k thermo-cycles. The failure modes were assessed. One-way and two-way analysis of variance (ANOVA) followed by the Tukey's multiple comparisons test was used for the statistical analysis.

Results

IP6 etching resulted in a more aggressive and uniform etching pattern compared with PAA. The mineral/matrix and Vickers microhardness of IP6-etched dentin were significantly less than those of PAA-conditioned dentin. IP6 etching significantly improved the resin−dentin SBS compared with the control group (no treatment) at 24 h and after thermo-cycling. Adhesive failures were the most predominant in all study groups.

Conclusion

Inositol hexaphosphate acid etching deteriorated dentin microhardness and resulted in substantial demineralization, however, it eliminated the dentin smear layer completely and created marked micromorphological alteration at dentin surface, significantly increasing the resin−dentin SBS of a self-adhesive restorative material.

本研究评估了 2% 肌醇六磷酸(IP6)和 10% 聚丙烯酸(PAA)对自粘修复材料(Surefil™ One;Dentsply Sirona,德国康斯坦茨)的牙本质表面微形态、基质/矿物质比、显微硬度和树脂-牙本质剪切粘接强度(SBS)的影响。用扫描电子显微镜(SEM)、共焦拉曼显微镜和使用维氏压头的显微硬度计分别对牙本质表面微形态(蚀刻模式)、基质/矿物质比率和显微硬度进行表征。将健全的臼齿切平、安装、表面处理并用 Dentsply 公司生产的 Surefil™ One 进行修复。使用万能试验机对 24 小时和 10k 热循环后的剪切粘接强度(SBS)进行评估。对失效模式进行了评估。统计分析采用了单因子和双因子方差分析(ANOVA)以及 Tukey's 多重比较检验。与 PAA 相比,IP6 蚀刻产生的蚀刻模式更强烈、更均匀。IP6 蚀刻牙本质的矿物/基质和维氏硬度明显低于 PAA 调理牙本质。与对照组(未处理)相比,IP6 蚀刻在 24 小时和热循环后可明显改善树脂-牙本质 SBS。在所有研究组中,粘合剂失效的情况最为普遍。肌醇六磷酸酸蚀刻会降低牙本质的微硬度并导致大量脱矿,但它能完全消除牙本质涂抹层并在牙本质表面产生明显的微观形态改变,从而显著提高自粘性修复材料的树脂-牙本质 SBS。
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引用次数: 0
Hydrothermal degradation behaviour of bonded joints using open-faced specimens 使用开口试样的粘接接头水热降解行为
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-07-27 DOI: 10.1016/j.ijadhadh.2024.103785

Moisture ingress into adhesive joints is known to reduce bond strength. The strength loss due to moisture is attributed to two primary causes. The first is the degradation of the adhesive layer, which progresses relatively slowly. The second is the reduction in the interfacial strength between the adhesive and the adherend, which is more difficult to predict. The degradation behaviour of interfacial strength varies depending on the adherend type. Therefore, the effect of water penetration on three open-faced steel and magnesium alloy specimens bonded with one-component epoxy adhesives was investigated. The open-faced specimen had no adherend on one side, and water penetrated at a high speed from the open side. The saturated water absorption state was reached faster in this specimen, which allowed the rapid confirmation of degradation after water absorption. To reduce test time, the specimens were examined in hot water at 87 °C. Initially, cohesive failure in adhesive layers occurred for the steel specimens and the strength decreased with time. Prolonged immersion resulted in progressive corrosion, and the fractures within the corrosion layer began to mix. For magnesium alloy plates, immersion in hot water caused immediate adhesion failure and, simultaneously, a significant reduction in the adhesion strength. When closed-faced specimens (i.e. normal specimens) were used instead of open-faced specimens, a sequential transition was observed from cohesion to adhesion failure with immersion from the edge.

众所周知,湿气进入粘合剂接缝会降低粘合强度。湿气导致的强度降低主要有两个原因。首先是粘合剂层的降解,其进展相对缓慢。其次是粘合剂与被粘物之间的界面强度降低,这一点较难预测。界面强度的降解行为因粘合剂类型而异。因此,我们研究了水渗入对使用单组分环氧树脂粘合剂粘合的三个开口钢和镁合金试样的影响。开口试样的一侧没有粘合剂,水从开口一侧高速渗入。这种试样更快达到饱和吸水状态,因此可以快速确认吸水后的降解情况。为了缩短试验时间,试样在 87 °C 的热水中进行了检验。最初,钢试样粘合层发生内聚破坏,强度随时间而降低。长时间浸泡导致逐渐腐蚀,腐蚀层内的裂缝开始混合。对于镁合金板,在热水中浸泡会导致粘合立即失效,同时粘合强度显著降低。当使用闭面试样(即普通试样)而不是开口试样时,可以观察到从边缘浸泡到粘附失效的顺序过渡。
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引用次数: 0
Thiolated nanoclays as a potential mucoadhesive material: Optimization by design of experiments and multivariate regression 硫醇化纳米粘土作为一种潜在的粘液黏附材料:通过实验设计和多元回归进行优化
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-07-26 DOI: 10.1016/j.ijadhadh.2024.103803

An integrated strategy based on design of experiments (DoE) and multivariate regression was carried out to produce an optimized surface functionalized nanoclay (Mt–SH) with potential mucoadhesive properties. A mercaptosilane was grafted in montmorillonite in order to immobilize thiol groups (–SH) on the clay. The functionalization was confirmed by IR, TGA, XRF and XRD analyses. Five variables involved in the synthesis were optimized in order to maximize two responses: mass of functionalized nanoclay and amount of thiol groups attached in the clay surface. This optimization was performed by a two–step DoE strategy using Plackett–Burman and Box–Behnken designs. The five variables and two responses were simultaneously calibrated in a single ANOVA–validated PLS regression model. Analyzing scores, loading and surface response plots, the main processing variables, interactions and quadratic terms were found achieving the optimal processing conditions for the synthesis. The quadratic model (R2 > 0.8589) predicted an optimized functionalized nanoclay of mass 3.29 ± 0.13 g of Mt–SH with 19.65 ± 0.78 μmol –SH per g Mt–SH (P < 0.05). The optimized Mt–SH was evaluated by in vitro and in situ mucoadhesion assays with porcine mucin and fresh intestinal mucus by using rheometry. The complex viscosity showed an increase of ∼54-fold higher compared to the unmodified Mt, and ∼12.8-fold increase in the elastic modulus, which indicates a more resistance to elastic deformation probably due to an increase in cross-linking points between Mt–SH and mucus. The formation of disulfide bonds between thiol groups from Mt–SH and glycoproteins in the mucin could be a reasonably explanation which shows a correlation respect other thiolated materials which show the same mucoadhesion properties. These results could project this functionalized silicate material as a potential mucoadhesive prospect for pharmaceutical applications.

研究人员采用基于实验设计(DoE)和多元回归的综合策略,制备出具有潜在粘液粘附特性的优化表面功能化纳米粘土(Mt-SH)。在蒙脱石中接枝了巯基硅烷,以便在粘土上固定硫醇基团(-SH)。通过红外光谱、热重分析、X射线荧光光谱和 X 射线衍射分析确认了功能化。对合成过程中涉及的五个变量进行了优化,以最大限度地提高两个响应:功能化纳米粘土的质量和粘土表面附着的硫醇基团的数量。优化采用了两步 DoE 策略,即 Plackett-Burman 和 Box-Behnken 设计。在一个经方差分析验证的 PLS 回归模型中同时校准了五个变量和两个响应。通过分析得分、载荷和表面响应图,发现主要加工变量、交互作用和二次项实现了合成的最佳加工条件。二次项模型(> 0.8589)预测出优化的功能化纳米粘土质量为 3.29 ± 0.13 克 Mt-SH,每克 Mt-SH 含 19.65 ± 0.78 μmol -SH(< 0.05)。利用流变仪对优化后的 Mt-SH 与猪粘蛋白和新鲜肠粘液进行了粘附试验。与未改性的 Mt 相比,复合物粘度增加了 54 倍,弹性模量增加了 12.8 倍,这表明 Mt-SH 与粘液之间的交联点增加了,因此抗弹性变形能力增强。Mt-SH的硫醇基团与粘蛋白中的糖蛋白之间形成的二硫键可能是一个合理的解释,这与其他具有相同粘附特性的硫醇材料相关。这些结果表明,这种功能化硅酸盐材料具有潜在的药物粘附性应用前景。
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引用次数: 0
Performance assessment of composite modified bitumen integrated with desulfurized crumb rubber and SBS modifier as waterproofing adhesive layer 以脱硫橡胶屑和 SBS 改性剂为防水粘合剂层的复合改性沥青性能评估
IF 3.2 3区 材料科学 Q2 ENGINEERING, CHEMICAL Pub Date : 2024-07-25 DOI: 10.1016/j.ijadhadh.2024.103802

Performance of the waterproofing adhesive layer played a critical role for governing duration of bridge deck paving system due to harsh service conditions. To develop a new type of modified bitumen suitable for the layer between bridge deck and overlaid asphalt, this study investigated the performance of composite modified bitumen (CMB) integrated with desulfurized crumb rubber (DCR) and SBS modifier. The influence of DCR and SBS additive on rheological behavior, high-temperature performance, low-temperature cracking resistance, and adhesive performance of CMB was investigated by adopting various experimental tests, which including penetration, ductility, softening point, Brookfield viscosity, dynamic shear rheometer (DSR), bending beam rheometer (BBR), and bonding strength. The high-temperature stiffness and low-temperature flexibility of CMB was improved after composite modification, which in turn contributed to the shear and cracking resistance. The black diagram indicated that the formation of polymer network in the CMB improved the viscous flow resistance and maintained elastic response at high in-service temperature. The bonding strength and moisture stability of the composite bitumen-concrete interface were enhanced, with the properties exceeded the commercial SBS modified bitumen. The CMB binders R18S2 and R18S3 presented good performance and can be used for waterproofing adhesive layer as a substitute of the commercial SBS modified bitumen.

由于使用条件苛刻,防水粘合层的性能对桥面铺装系统的使用寿命起着至关重要的作用。为了开发一种适用于桥面铺装和沥青面层之间的新型改性沥青,本研究对添加了脱硫橡胶(DCR)和 SBS 改性剂的复合改性沥青(CMB)的性能进行了研究。通过各种实验测试,包括渗透性、延展性、软化点、布鲁克菲尔德粘度、动态剪切流变仪(DSR)、弯曲梁流变仪(BBR)和粘结强度,研究了脱硫橡胶和 SBS 添加剂对 CMB 的流变行为、高温性能、低温抗裂性和粘结性能的影响。复合材料改性后,CMB 的高温刚度和低温柔度得到改善,从而提高了抗剪切和抗开裂性能。黑色图表显示,CMB 中聚合物网络的形成改善了粘流阻力,并保持了在高使用温度下的弹性响应。复合沥青-混凝土界面的粘结强度和湿稳定性得到了提高,其性能超过了商用 SBS 改性沥青。CMB 粘结剂 R18S2 和 R18S3 具有良好的性能,可替代 SBS 改性沥青用于防水粘结层。
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引用次数: 0
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International Journal of Adhesion and Adhesives
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