加成型有机硅灌封胶的粘接性能研究

以杂氮硅三环衍生物为增粘剂,制备了加成型粘接有机硅灌封胶。研究了导热填料用量、导热填料处理方式、增粘剂用量以及A值(硅氢基与硅乙烯基摩尔比)对加成型有机硅灌封胶粘接性能影响。结果表明,当导热填料硅微粉用量150份、导热填料硅微粉采用A171表面处理、增粘剂用量2.0份、A值1.4时,制备出对铝材、PA、ABS、PC粘接性能良好且导热、阻燃等综合性能优异的加成型有机硅灌封胶。     

绝缘导热加成型有机硅灌封胶的制备及性能研究

研究绝缘导热加成型有机硅灌封胶的制备及性能。结果表明:当采用粘度为300和1 000 m Pa·s的端乙烯基硅油以质量比40∶60复配、选用活性氢质量分数为0.005 0的含氢硅油且硅氢基/硅乙烯基摩尔比为1.2时,有机硅灌封胶的物理性能较佳;当三氧化二铝用量为150份时,有机硅灌封胶具有良好的综合性能。     

加成型导热电子灌封胶的研制

以端乙烯基硅油为基胶、含氢硅油为交联剂、α-Al2O3和氮化硼(BN)为导热填料制得加成型导热灌封胶。研究了导热填料的种类、用量和配比对灌封胶导热性能的影响。结果表明:α-Al2O3的导热系数最大;随着BN用量的增加,灌封胶的导热系数和拉伸强度提高,断裂伸长率先增后降,但粘度上升明显。不同粒径的α-Al2O3和氮化硼(BN)并用可以提高灌封胶的导热系数,且对粘度和力学性能影响较小。     

导热有机硅电子灌封胶的制备与性能研究

采用端乙烯基硅油为基胶、含氢硅油为交联剂、三氧化二铝(Al2O3)为导热填料,制备了导热有机硅电子灌封胶。研究了Al2O3的粒径及用量、不同粒径Al2O3并用和硅烷偶联剂对灌封胶性能的影响。结果表明,Al2O3的粒径越大,灌封胶的热导率越大,但拉伸强度和扯断伸长率减小,适合的Al2O3粒径为5μm或18μm;随着Al2O3用量的增加,灌封胶的热导率、拉伸强度增大,扯断伸长率先增后减,但黏度上升,Al2O3适合的加入量为150～200份;将不同粒径的Al2O3并用填充到灌封胶中可以提高灌封胶的热导率,当18μm Al2O3和5μm Al2O3的质量比为120∶80时,灌封胶的热导率达到0.716 W/(m.K),且对灌封胶的黏度和力学性能基本没影响;加入KH-570可改善灌封胶的力学性能,但热导率有所下降,适宜的用量为Al2O3质量的0.5%。     

高导热低黏度环氧树脂灌封胶

以E-51型环氧树脂为基体,Al2O3为导热填料,CYH-277为稀释剂制备高导热低黏度环氧树脂灌封胶。优化了硅烷偶联剂KH-560、稀释剂CYH-277的用量;分别采用NDJ-7型旋转式黏度计和Hot Disk型热常数分析仪测试其黏度和导热系数。结果表明:硅烷偶联剂KH-560用量为1.25%(wt)时效果最优;随CYH-277用量的增加灌封胶黏度、耐热性能均逐渐下降,最佳用量为25%(wt);随Al2O3用量增加,灌封胶的黏度、导热系数均增大;用量相同时,填充20μm Al2O3的树脂体系相比于填充6μm Al2O3树脂体系黏度小、导热系数大,复配两种粒径Al2O3对应树脂体系的导热性最好;复配Al2O3用量为86%(wt)时,导热系数达到2.23W/(m·K),此时灌封胶的黏度为30100mPa·s,仍保持较好的加工流动性。     

氢氧化铝对有机硅电子灌封胶性能的影响

以端乙烯基硅油为基胶、含氢硅油为交联剂、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)为表面处理剂、Al(OH)3或Al(OH)3/铂络合物为阻燃剂,制备阻燃型有机硅电子灌封胶。研究结果表明:对Al(OH)3表面进行处理、降低其粒径、增加其含量、Al(OH)3/铂络合物并用等均有利于提升灌封胶的阻燃性能;当w(KH-570)=0.5%[相对于Al(OH)3质量而言]、Al(OH)3的平均粒径为2.6μm、m(5.0μmAl2O3):m[2.6μm Al(OH)3]=160:40和w(铂络合物)=0.002%(相对于基胶质量而言)时,可制得阻燃性优异的有机硅电子灌封胶。     

单组分加成型导热有机硅橡胶的制备

采用端乙烯基硅油为基胶,低含氢硅油为交联剂,氯铂酸-异丙醇为硫化剂,三氧化二铝（A12O3）为导热填料,制备了单组分导热有机硅电子灌封胶;讨论了1-乙炔基环己醇、乙烯基环体和苯乙炔对单组分灌封胶储存稳定性的影响,研究了不同粒径A12O3颗粒配比和用量对灌封胶导热系数和粘度的影响。结果表明,1-乙炔基环己醇抑制效果较好,当其用量为2.2份时单组分硅橡胶室温储存期为3个月;A12O3用量越大,硅橡胶导热系数越高,粘度越大,不同粒径A12O3互配使用可提高硅橡胶导热系数,当8μm和3μmA12O3质量比为3∶1,填料总用量为240份时,制得导热系数为0.822W/（m.K）单组分有机硅灌封胶。     

无机填料粒子的几何特征对环氧树脂灌封胶导热性能的影响

以Al2O3、Si3N4、BN、SiO2和AlN五种无机填料作为环氧树脂(EP)灌封胶的导热填料,研究了填料的种类、粒径大小和颗粒形态等对EP灌封胶热导率的影响。结果表明:EP灌封胶的热导率随着导热填料用量的增加而增大;当φ(BN)=35%(相对于总体积而言)时,相对最大热导率为2.12 W/(m·K),其值约为EP基体的10倍。填料粒子的几何特征对EP灌封胶的导热性能具有较大的影响;当Al2O3粒径为48μm时,EP灌封胶的相对最大热导率为1.3 W/(m·K);填料粒子过大或过小都会降低EP灌封胶的导热性能。层片状填料粒子可以获得较大的堆积密度,在EP灌封胶中能有效形成导热通道,增加其热导率。     

ZnO在Al_2O_3/导热环氧树脂灌封胶中的应用研究

采用硅烷偶联剂KH-560对ZnO粉体表面改性,研究了ZnO粒径及用量对Al2O3/导热环氧树脂灌封胶导热系数、粘度、拉伸剪切强度、沉降率、触变指数、耐热性的影响。结果表明:表面改性后的ZnO粉体颗粒分散均匀,无明显团聚现象;相同用量时,填充0.5μm ZnO的树脂体系的综合性能较5μm ZnO体系好。随ZnO用量的增加,灌封胶的导热系数、拉伸剪切强度、触变指数均呈先增大后减小的趋势,ZnO添加质量分数为20%时灌封胶导热系数、拉伸剪切强度最大,分别为0.84 W/(m·K)、16.78 MPa,ZnO添加质量分数为60%时触变指数最大为1.89。随ZnO用量的增加灌封胶的粘度、耐热性均逐渐增大,沉降率逐渐降低。     

空心玻璃微珠在有机硅灌封胶中的应用

将不同真密度和粒径的空心玻璃微珠(HGS)用于填充加成型硅橡胶，制得低密度、低导热有机硅灌封胶。考察了不同种类空心玻璃微珠对有机硅灌封胶密度、黏度、热导率等的影响。在HGS体积分数相同的条件下，真密度小的HGS有助于获得更低密度的有机硅灌封胶，但HGS的粒径对有机硅灌封胶密度的影响很小；随着HGS真密度的增大，有机硅灌封胶的黏度也逐渐增大。对于相同真密度不同粒径的HGS,其粒径减小时，灌封胶的黏度略有增大；HGS的真密度对有机硅灌封胶热导率的影响不明显，但相同真密度的HGS,粒径大的HGS填充的有机硅灌封胶热导率偏小。     

高导热阻燃有机硅灌封胶的制备

以乙烯基硅油、含氢硅油为基础胶料,十六烷基三甲氧基硅烷改性氧化铝为导热填料,二乙基次膦酸铝(ADP)为阻燃剂,制得导热阻燃绝缘有机硅电子灌封胶。研究了改性氧化铝用量对灌封胶黏度、导热性、阻燃性的影响,观察了燃烧残余物的形貌。结果表明,这种改性氧化铝有低吸油值,填充量对灌封胶黏度影响小,所制备的灌封胶具有良好导热性能;而ADP不仅展现出对灌封胶良好的阻燃性,而且还能与改性氧化铝产生协效阻燃性和抑烟作用,同时灌封胶也具有良好的流动性、力学性能和电绝缘性能。当ADP用量50份、改性氧化铝用量600份时,灌封胶的黏度为8 500 mPa·s,硫化后胶条的热导率达2.12 W/m·K,垂直燃烧达到FV-0级,拉伸强度1.72 MPa,拉断伸长率62%,体积电阻率3.9×1012Ω·cm。     

Synthesis of silane oligomers containing vinyl and epoxy group for improving the adhesion of addition-cure silicone encapsulant

Two types of silane oligomers containing vinyl and epoxy group (PTGM and PTGE) as adhesion promoters were synthesized by the reaction of trimethylolpropane monoallyl ether with 3-glycidoxypropylmethyldimethoxysilane and 3-glycidoxypropylmethyldiethoxysilane, respectively. Fourier transform infrared spectroscopy, ¹H nuclear magnetic resonance spectroscopy, and gel permeation chromatography were used to characterize their chemical structures. The effect of adhesion promoters on properties of addition-cure silicone encapsulant (ASE) with lots of alumina (Al₂O₃) particles as thermally conductive fillers was investigated. The results showed that PTGM and PTGE could significantly improve both the adhesive strength and mechanical properties of ASE. The viscosity of ASE with no more than 3.0 phr PTGM and PTGE was below 5000 mPa s so that they were suitable for encapsulating process. Observation using scanning electron microscopy revealed that PTGM and PTGE could improve the dispersion of Al₂O₃ particles in silicone rubber matrix and enhance the bond between the particles and the matrix.     

自粘性加成型阻燃导热有机硅电子灌封胶的研制

采用端乙烯基硅油、含氢硅油为基料,氧化铝为导热填料,氢氧化铝为阻燃剂,乙烯基三甲氧基硅烷及γ-甲基丙烯酰氧基丙基三甲氧基硅烷的混合物为偶联剂,铂配合物为催化剂,三羟甲基丙烷二烯丙酯、γ-环氧丙氧丙基三甲氧基硅烷及正硅酸乙酯的反应产物作增粘剂,制备了双组分加成型阻燃导热有机硅电子灌封胶。结果表明,较佳配方为:100份端乙烯基硅油、8份含氢硅油(活性氢质量分数0.25%)、铂的质量分数15×10-6、0.05份抑制剂、150份氧化铝、30份氢氧化铝、0.5份偶联剂、3份增粘剂,所得灌封胶无需底涂剂、在90℃的加热条件下可对PC和铝材等有良好的粘接性,热导率0.8W/m.K,阻燃等级UL94V-0,能够满足大功率电子元器件的灌封要求。     

A study of the flame‐retardant properties of polypropylene/Al(OH)3/Mg(OH)2 composites

Polymeric materials are used extensively, but their applications are limited because many of them are flammable. Therefore ways to make them flame retardant have received much attention. In this work, polypropylene (PP) was used as the matrix resin, aluminium hydroxide (Al(OH)₃) and magnesium hydroxide (Mg(OH)₂) as flame‐retardant additives and zinc borate (ZB) as a flame‐retardant synergist. PP/Al(OH)₃/Mg(OH)₂ and PP/Al(OH)₃/Mg(OH)₂/ZB flame‐retardant composites were prepared with a twin‐screw extruder. The flame‐retardant properties, i.e. oxygen index (OI), burning velocity and smoke density, of the composites were measured. The results showed that OI increased with an increase of the filler content and decreased with an increase of the filler particle diameter. The burning velocity decreased with an increase of the filler content, while it first increased and then decreased with an increase of the filler particle diameter. The smoke density decreased with an increase of the filler content and increased with an increase of the filler particle diameter. There was a flame‐retardant synergy between Al(OH)₃/Mg(OH)₂ and ZB in the composites, and the smoke suppression effect was marked when ZB was added. Copyright © 2009 Society of Chemical Industry     

加成型阻燃导热有机硅电子灌封胶的研制

以乙烯基硅油、舍氢硅油为基料,铂络舍物为催化剂制得双纽分加成型有机硅灌封胶。通过添加导热和阻燃填料提高灌封胶的导热性和阻燃性,加入增粘剂改善有机硅的粘接性能。结果表明,100份乙烯基硅油（乙烯基质量分数1％）中含氢硅油（活性氢质量分数0.18％）15份、铂含量10×10^-6、导热填料40份、阻燃剂含量50×10^-6、增粘剂1份,所得灌封忮具有较好的综合性能,能够满足大功率电子元器件的灌封要求。     

新型氢氧化物阻燃剂在胶粘剂领域中的应用进展

介绍了表面改性、超细化、以及与其他阻燃剂联用等途径对氢氧化物[Al(OH)3、Mg(OH)2]阻燃性能的影响,综述了新型阻燃剂在胶粘剂领域中的应用研究进展,比较了氢氧化物、改性氢氧化物、氢氧化物协同作用、氢氧化物和有机物协同作用等对各种胶粘剂阻燃性能和力学性能的改进效果,讨论了该领域研究中依然存在的一些不足,指出了今后的研究可能取得突破的几个方向。     

Synthesis of phenyl silicone resin with epoxy and acrylate group and its adhesion enhancement for addition-cure silicone encapsulant with high refractive index

A novel phenyl silicone resin with epoxy and acrylate group (PSREA) was successfully synthesized via the non-hydrolytic sol-gel condensation reaction of 3-glycidoxypropyltrimethoxysilane, 3-methacryloyloxypropylmethyldimethoxysilane, and diphenylsilanediol, and was employed as the adhesion promoter for addition-cure silicone encapsulant (ASE) with high refractive index. The structure of PSREA was confirmed by Fourier transform infrared spectroscopy, ¹H nuclear magnetic resonance spectroscopy, and ²⁹Si nuclear magnetic resonance spectroscopy. The influence of PSREA on the properties of ASE was studied. It was found that PSREA could markedly enhance the adhesion strength of ASE to aluminum (Al) and poly(p-phenylene terephthamide) (PPA) substrate. When the content of PSREA was 1.5 phr, the shear strength of ASE was 4.43 and 2.27 MPa for Al and PPA substrate, which was about 71 and 266% higher than that of ASE without the adhesion promoter, respectively. In addition, PSREA had little effect on the mechanical properties, refractive index, and viscosity of ASE.     

阻燃剂对聚氨酯阻尼涂料性能的影响

通过在聚氨酯涂料中添加氢氧化铝[Al(OH)₃]、可膨胀石墨(EG)、三(2-氯异丙基)磷酸酯(TCPP),制备了兼具阻尼与阻燃性能的聚氨酯阻尼涂料。研究了3种阻燃剂对涂料力学性能、阻燃性能与阻尼性能的影响,研究结果表明:Al(OH)₃能提高材料的力学性能和阻燃性能,温度较低时,能提高阻尼性能,温度较高时,将降低阻尼性能;适量的EG能够显著提高材料阻燃性能与阻尼性能;TCPP可以提高材料的断裂伸长率,在添加量较少时,显著提高材料的阻燃性能,但材料阻尼性能有所降低。     

Thermal behavior and flame retardancy of flexible poly(vinyl chloride) treated with Al(OH)3 and ZnO

Al(OH)₃ as flame retardant and smoke suppressant for flexible poly(vinyl chloride) was evaluated alone and with ZnO, using thermal analytical techniques, limiting oxygen index and smoke density rating tests. The thermal behavior and flammability of the samples treated with Al(OH)₃ and ZnO were studied by differential thermal analysis and thermogravimetric analysis. The activation energy was calculated by using the Vyazovkin model‐free kinetic and Kissinger methods. The results showed that the flame‐retardant and smoke‐suppressant properties of the samples treated with Al(OH)₃ and ZnO were related to the content of ZnO and the thermal effect during the process of thermal degradation of the samples. Copyright © 2005 Society of Chemical Industry     

卡拉胶-纳米氢氧化铝协同阻燃天然橡胶

将BaCl2分级的k型卡拉胶(KC)和纳米氢氧化铝〔Al(OH)3〕构成的协同阻燃体系添加到天然橡胶(NR)中制备KC-Al(OH)3/NR复合材料。通过TG、极限氧指数(LOI)、锥形量热(CCT)以及SEM考察了不同质量比的KC和Al(OH)3对复合材料力学性能和阻燃性能的影响。结果表明,当KC与Al(OH)3以1∶1的质量比加入到NR时,KC-Al(OH)3/NR复合材料的热稳定性、阻燃性能最优,复合材料的LOI达到25%。与纯天然橡胶相比,复合材料总热释放量(THR)、热释放速率峰值(pHRR)、总烟释放量(TSP)和平均质量损失率(AMLR)分别降低了12%、65%、23%和62%。相比于单独添加Al(OH)3体系,复合材料拉伸强度和断裂伸长率分别增加了11%和17%。