填充碳纳米管各向同性导电胶的性能

制备了以碳纳米管(CNTs) 和镀银碳纳米管(SCCNTs) 为导电填料的各向同性导电胶, 研究了它们的电学性能、力学性能及抗老化性能, 并与传统的以微米量级的银粒子作为导电填料的导电胶的性能进行比较。研究发现: CNTs 作为导电填料时, 在填料体积分数为31 %时出现体积电阻率的最低值2. 4 ×10-3Ω·cm; 在填料体积分数为23 %时导电胶表现出最好的抗剪切性能。在填料体积分数同为28 %时, 填充SCCNTs 导电胶具有最低的体积电阻率2. 2 ×10-4Ω·cm; 填充CNTs 和SCCNTs 显示出比填充微米量级银粒子导电胶高的抗剪切强度(19. 6 MPa) 。在85 ℃、RH 85 %环境下经过1000h 老化测试结果表明: 填充SCCNTs 或CNTs 导电胶体积电阻率的变化和剪切强度的变化均不超过10 %; 而填充微米量级银粒子导电胶在老化后体积电阻率的变化和抗剪切强度的变化分别达到350 %和120 %。      

低温快速固化环氧导电胶的制备与性能

采用E-51型环氧树脂为导电胶基体树脂, 低分子量聚酰胺树脂(PA)为固化剂, 填加经硅烷偶联剂(KH550)改性后的纳米级和微米级铜粉及助剂制备导电胶。首次采用了液态固化剂(低分子量的聚酰胺酯), 以解决导电胶制备过程中填料用量受限的难题。通过正交试验方法探讨了导电胶中导电填料的含量、导电填料配比、硅烷偶联剂用量和还原剂添加量对导电胶粘接性能和导电性能的影响, 对导电胶的制备工艺进行了优化, 获得了制备导电胶的最佳方案。测试结果表明该导电胶能够在60 ℃下4 h内快速固化。在填料质量分数为65%时, 导电胶具有最低的体积电阻率3.6×10-4 Ω·cm; 导电胶的抗剪切强度达到17.6 MPa。在温度为85 ℃、湿度(RH)为85%的环境下经过1000 h老化测试后导电胶电阻率的变化和剪切强度的变化均不超过10%。      

填充银纳米棒新型导电油墨

采用微波辅助原位氧化还原法制备长径比均匀的银纳米棒, 研究了制备条件参数如催化剂浓度、 表面活性剂与先驱体浓度比率等因素对制备银纳米材料的形貌的影响。以这些银纳米棒作为导电填料制备印刷用导电油墨, 研究了填料含量、 纳米棒及纳米粒子的比率对导电油墨的电导率、 附着力、 老化性能的影响。结果表明, 当晶体生长催化剂NaCl与AgNO₃的摩尔比为1:5时, 得到的银纳米材料中纳米棒比例达95%以上。对导电油墨的性能研究表明, 当填料中银纳米棒比例为95%时得到的导电胶具有最低的渗滤阈值, 为62%, 同时经过80℃、 85%RH老化环境老化500 h后导电油墨的体积电阻率上升不超过10%。     

填料长径比对导电胶渗流阈值的影响

采用微波辅助乙二醇还原法制备了不同长径比的银纳米方块及银纳米线, 并对其进行了SEM、 XRD表征。以不同长径比银纳米线作为导电填料制备了各向同性导电胶。对导电胶的填充渗流阈值的研究发现, 填料的长径比对填充渗流阈值的影响很大, 长径比越大, 渗流阈值越小。运用修正的阈值理论对这一实验现象进行了合理解释, 模拟结果表明修正的阈值理论与实验结果非常吻合。      

新型纳米银导电胶的制备及其性能研究

通过液相化学还原法制备纳米银粉,经扫描电子显微镜(SEM)和X射线衍射(XRD)表征,表明该方法制备的纳米银粉纯净,粒度分布均匀,呈短棒状.该纳米银粉作为导电填料加入可以有效地改善导电胶体系的体积电阻率和连接强度.在总银粉填充量60%,纳米银粉与微米银粉比例为1:5的情况下,导电胶的体积电阻率达到最低值1.997×10-4Ω·cm,同时连接强度达到18.9MPa.     

SiO2 / 氰酸酯纳米复合材料的力学性能和热性能

采用高速均质剪切法制备了SiO₂ / 氰酸酯(CE) 纳米复合材料, 并对该体系的静态力学性能、动态力学性能和热稳定性进行了研究。结果表明, 纳米SiO₂的加入提高了复合材料的冲击强度和弯曲强度。当SiO₂ 含量为0. 30 wt %时, 复合材料的冲击强度达最大, 增幅为88. 9 %; 当SiO₂含量为0. 15 wt %时, 材料的弯曲强度达最大, 增幅为2010 %。复合材料的储能模量和高温损耗模量较纯CE 树脂有明显提高, 玻璃化转变温度比纯CE 提高了31. 2 ℃, 热分解温度在SiO₂含量为0. 30 wt %时达最大, 失重为10 %时的热分解温度提高了25. 7 ℃。      

银纳米线-聚对苯二甲酸乙二醇酯透明导电胶膜

以银纳米线作为导电填料,以聚对苯二甲酸乙二醇酯(PET)为柔性衬底,采用平板热压机通过热压方式制备了银纳米线-PET透明导电胶膜。研究了银纳米线-PET导电胶膜的耐弯曲性能、电学性能以及透光性。结果表明,所制备的银纳米线-PET导电胶膜透光率达到80%以上,表面电阻率达到1×10^-3Ω·cm。银纳米线-PET导电胶膜经过500次的弯曲循环后电阻率未下降。随着银纳米线溶液浓度的增加,银纳米线-PET导电胶膜透光性下降,表面电阻率增加。     

银纳米线/聚乙烯醇导电复合材料的逾渗特性研究

采用多元醇法制备了长径比约为240的银纳米线(AgNWs),以聚乙烯醇(PVA)为基体、AgNWs为导电填料制备了导电复合材料;基于排斥体积理论和几何相变理论对银纳米线/聚乙烯醇导电复合材料的逾渗阈值进行了分析和预测。结果表明,基于排斥体积理论计算得到的逾渗阈值(0.5816%)小于实际复合材料的实测数据;基于几何相变理论模型对材料逾渗阈值的拟合数据约为1.25%～1.31%,与实验测试得到的复合材料逾渗转变浓度范围一致性较好。因此,利用几何相变理论进行复合材料逾渗阈值和电导率的预测对于AgNWs/PVA导电复合材料的设计、制备及性能评价具有重要的指导作用。     

石墨烯多壁碳纳米管/超高分子量聚乙烯导电复合材料的制备及性能

为了比较超高分子量聚乙烯(UHMWPE)在单一填充和混合填充时, 复合材料导电性的差别。在超声和肼的作用下, 通过对氧化石墨烯(GO)、 多壁碳纳米管(MWCNTs)和超高分子量聚乙烯水/乙醇分散液减压蒸馏及热压制备了隔离型MWCNTs/UHMWPE、 石墨烯(GNS)/UHMWPE和MWCNTs-GNS/UHMWPE导电复合材料。经SEM、 TEM测试发现, 导电填料分散于UHMWPE颗粒表面, 热压后形成隔离结构。隔离型的MWCNTs/UHMWPE和GNS/UHMWPE复合材料均表现出较低的导电逾渗(0.148%和0.059%, 体积分数,下同), 但MWCNTs/UHMWPE复合材料的电导率(2.0×10^-2 S/m, 1.0%, 质量分数, 下同)明显高于相同填料含量下的GNS/UHMWPE复合材料。 MWCNTs-GNS/UHMWPE复合材料表现出了更低的逾渗(0.039%) 和较高导电性能(1.0×10^-2 S/m, 1.0%), 其拉伸强度和断裂伸长率随填充剂含量的增加呈现出先上升后下降的趋势。     

原位复合法制备TiO2 / ( PEO)8LiClO4 聚合物电解质

以聚氧化乙烯/ 高氯酸锂络合物( ( PEO)₈LiClO₄ ) 为基体, 通过钛酸四丁酯的水解缩合反应在基体中原位生成TiO₂粒子, 制备了TiO₂ / ( PEO)₈LiClO₄复合聚合物电解质膜。采用SEM、DSC 和交流阻抗方法分别研究了电解质膜的表面形貌、热性能和离子导电性能。结果表明, 原位生成的TiO₂ 粒子均匀分散于PEO 基体中。复合TiO₂后电解质膜的玻璃化转变温度和结晶度降低。电解质膜的离子导电行为满足Arrhenius 方程, 并在5 %TiO₂含量时体系的电导率出现最大值5. 5 ×10 -5 S/ cm (20 ℃) 。以此膜为电解质组装的全固态聚合物锂电池放电时电压平稳, 20 次循环后放电容量保持在107 mAh/ g。      

纳米Ag链的制备及其在聚氨酯基柔性导电复合材料中的应用

针对柔性聚合物基导电复合材料的导电性差和柔性差这2个关键问题,分别从导电填料的柔性化及降低填料含量2方面着手,以脱氧核糖核酸（DNA）大分子链作为模板,制备了大小均一、链状排列的柔性纳米Ag链及纳米Ag链填充的聚氨酯基柔性导电复合材料。利用SEM对纳米Ag链/Ag包Cu粉/聚氨酯导电复合材料的界面结构进行了表征,探讨了纳米Ag链/Ag包Cu粉/聚氨酯导电复合材料导电性及柔性的机制。研究发现:保持导电填料总质量分数为76%、纳米Ag链的质量分数为4%时,纳米Ag链/Ag包Cu粉/聚氨酯导电复合材料的电阻率及形变前后的电阻变化比值达到最佳值,分别为2.13×10-4 Ω·cm和3.6;当以纳米Ag链为单一填料时,制得的纳米Ag链/聚氨酯导电复合材料具有优异的柔性;泡沫法制备的纳米Ag链/聚氨酯导电复合材料可以在低填料质量分数时达到更高的导电性,当纳米Ag链质量分数为60%时,方阻为56 Ω/sq,低于共混法制备的填料质量分数为65%时的纳米Ag链/聚氨酯导电复合材料（98 Ω/sq）。      

One step synthesis of silver nanowires used in preparation of conductive silver paste

For mass preparation of conductive silver paste, a convenient approach to synthesize silver nanowires (Ag NWs) is presented. Monodisperse Ag NWs with ca. 40 nm in diameter and over 10 μm in length were successfully obtained in high yield only by heating a mixture of AgNO₃, poly(vinyl pyrrolidone), ethylene glycol and HCl prepared previously. This method not only simplifies the conventional polyol process but also extremely improves its repeatability. More important, the patterns fabricated with the Ag NWs naturally have a high conductivity, up to ca. 13 % of bulk silver, due to the cross-linked network structure formed by accumulation of nanowires. The conductivity even can be improved to 41 % of bulk silver conductivity through a chemical sintering at room temperature, which makes us believe that the Ag NWs could be broadly applied in preparation of conductive paste.     

Isotropical conductive adhesives with very-long silver nanowires as conductive fillers

Isotropical conductive adhesives (ICAs) have garnered great attention from the researchers in electronic industry as a potential substitute to lead-bearing solders for novel microsystem. In this paper, silver nanowires with a diameter of approximately 390 nm and a length of over 100 μm were synthesized by a polyol process. The ICAs composed of an epoxy-based binder containing silver nanowire were prepared and the curing behaviors, electrical properties, hygroscopicity, and the tensile shear strength of ICAs were investigated. Silver nanowires affect the curing behavior of epoxy resin and reduce the cross-linking density. The resistivity of the ICAs filled with 10, 35 and 45 wt% silver nanowire cured at 150 °C is 8.9 × 10^?3, 1.69 × 10^?5 and 4.9 × 10^?6 Ω cm respectively. The resistivity of the ICAs filled with silver nanowire cured at 150 °C is little change after aged under 85 °C/85 % for 264 h. With the increase of the loading of silver nanowire the tensile shear strength of the ICAs increase. The reasons for the effects of silver nanowires on the curing behavior and the electrical property and hygroscopicity and the tensile shear strength were discussed in terms of the morphology, distribution, and higher activity of silver nanowires.     

Characterization of SiO2/Ag composite particles synthesized by in situ reduction and its application in electrically conductive adhesives

In the study, SiO₂/Ag composite particles with silver coating onto the surface of silica have been successfully prepared via a novel and facile approach (Oxidation–Reduction Method). In this approach, the SiO₂ particles were first modified with 3-ammoniatriethoxysilane (APTES) and glyoxalic acid (GA) through two-step reaction, the aldehyde group (CHO) were anchored onto the surfaces of silica spheres via electrostatic attraction, these [Ag(TEA)₂]⁺ ions in the solution were then reduced by the CHO and coated onto the surface of silica to obtain SiO₂/Ag composite particles. The effects of the reaction conditions on silver content and synthetic mechanism had also been discussed. The structure, morphology and optical properties of the SiO₂/Ag composite particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV–vis spectroscopy. The results showed the surface of SiO₂ was surrounded by pure silver nanoparticles, and the silver nanoparticles had face-centered-cubic structure, the SiO₂/Ag composite particles with core–shell morphology and special optical properties. And the small content SiO₂/Ag composite particles applied in electrically conductive adhesives (ECAs) improved the electrical bulk resistivity and tensile shear strength.     

Conductivity improvement of silver flakes filled electrical conductive adhesives via introducing silver–graphene nanocomposites

In this study, silver–graphene nanocomposites (SGNs) were successfully prepared by spontaneous reduction of silver ions and graphene oxide. Silver nanoparticles (about 30 nm) with narrow size distribution were distributed randomly on the surface of graphene. Different amounts of SGNs were introduced into silver flakes filled electrical conductive adhesives (ECAs) to study the effect of SGNs on the properties of the ECAs. The results showed that the volume resistivity of the ECAs decreased first and then increased with the increase of weight ratios of SGNs to silver flakes. While the weight ratio of SGNs to silver flakes was 20:80 (%), the resistivity reached the lowest value of 2.37 × 10^?4 Ω cm. The lap shear strength decreased with the increase of the content ration of SGNs. And when the weight ratio of SGNs to silver flakes was 20:80 (%), the lap shear strength of ECA was about 10 MPa. According to the thermogravimetric analysis, the addition of SGNs can cause a slight decrease in the thermal stability of the ECA. In summary, SGNs are the promising candidates for the conductivity improvement of silver flakes filled electrical conductive adhesives.     

Effects of hybrid fillers based on micro- and nano-sized silver particles on the electrical performance of epoxy composites

In the present study, electrically conductive adhesives produced from hybrid fillers based on micro- and nano-sized silver (Ag) was developed. The influence of the hybrid filler composition on the electrical properties of the hybrid system was studied. The electrical conductivity of the epoxy composites filled with micro- and nano-silver was correlated with their morphologies. A positive effect was observed in the electrical conductivity result when the composition of micro- and nano-sized Ag particles reached a 50:50 weight ratio. The nano-sized Ag particles became interconnecting particles in the interstitial spaces between micro-sized particles. Micrograph scanning shows that the particles were well distributed and dispersed, the separation between lumps of Ag filler by the insulating matrix was significantly reduced, leading to the formation of continuous linkages. The increased electrical conductivity resulted in a charge around the particle distribution, which led to the high capacity. Hence, these particles increased the conductivity of the system.     

Preparation of highly conductive adhesives by in situ generated and sintered silver nanoparticles during curing process

The lower resistivity (7.5 × 10⁻⁵ Ω cm) of nano-electrically conductive adhesives (nano-ECAs) with silver flakes and in situ formed and sintered silver nanoparticles was developed. At room temperature,the silver nanoparticles (Ag NPs) could not be generated in ECAs due to no reaction between silver nitrate and N,N-dimethyl-4-aminobenzaldehyde (DABA). However, during curing process, Ag NPs were immediately generated through reducing silver nitrate by DABA in absence of stabilizing agents. At the same time, the increased viscosity of epoxy due to the curing could prevent the agglomerates of Ag NPs. Morphology studies showed that most Ag NPs have been attached onto the surfaces of silver flakes due to the good affinity between them, resulting in more effectively interconnecting with silver flakes by the sintered Ag NPs. Thus, the lower bulk resistivity was obtained. On the other hand, DABA, containing a tertiary amine, can stabilize contact resistance of nano-ECAs by effectively preventing galvanic corrosion at the interface between nano-ECAs and Sn surfaces due to the fact that amines can strongly bond to a Sn surface.