低介电阻燃型氰酸酯胶黏剂的制备与性能研究

发布时间：2018-01-27 23:39

本文关键词： 介电性能阻燃性能粘接性能固化性能热稳定性氰酸酯胶黏剂　出处：《西南科技大学》2017年硕士论文　论文类型：学位论文

【摘要】：氰酸酯树脂(CE)具有卓越的介电性能、较高的粘接性能、优异的阻燃性能、较高的耐热温度和热稳定性等优异的性能,使得CE成为了许多尖端领域(如航空航天材料、电子信息材料和电绝缘材料等)的基体树脂材料。但是CE的自催化固化温度高(Tg),且固化时间长,而许多电子元器件不能承受这种固化温度和固化时间,另外,聚氰酸酯中没有反应的—OCN会严重影响其介电性能;与此同时,普通氰酸酯的阻燃特性已经不能满足现代材料日益增长的阻燃性能要求。因此,近年来,制备固化性能好、介电性能优异且阻燃性能出色的氰酸酯胶黏剂已经受到了广大研究者的关注。本文分别以双酚AF(BPAF)、双酚AF型环氧树脂(DGEBHF)和10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO-HQ)改性双酚A型氰酸酯(BACY),制备低介电阻燃型氰酸酯胶黏剂,并详细地研究了它们的性能。(1)用BPAF改性BACY,制备低介电阻燃型氰酸酯胶黏剂。首先,通过凝胶时间(GT)、差示扫描量热法(DSC)和傅里叶变换红外光谱(FT-IR)分析了BPAF/BACY胶黏剂的固化性能,结果发现,BPAF能显著改善BACY的固化性能。通过与壬基酚(No P)/BACY胶黏剂和双酚A(BPA)/BACY胶黏剂对比发现:BPAF/BACY胶黏剂具有更优异的性能。另外,详细地研究了BPAF添加量对BPAF/BACY胶黏剂性能的影响,结果表明,BPAF的最佳添加量为体系总质量的15%,此时BPAF/BACY胶黏剂的介电常数(Dk)为2.68,介电损耗角正切值(Df)为0.0081,极限氧指数(LOI)为35.8%。(2)用DGEBHF改性BACY,制备低介电高韧性氰酸酯胶黏剂,并对比双酚A型环氧树脂(DGEBA)/BACY胶黏剂研究了其性能。采用GT、DSC和FT-IR分析了DGEBHF对BACY胶黏剂固化性能的影响,结果表明,DGEBHF能有效改善BACY胶黏剂的固化性能。通过胶黏剂固化物性能分析可得,添加相同比例的环氧时,DGEBHF/BACY胶黏剂的性能明显优于DGEBA/BACY胶黏剂;当DGEBHF/BACY=15/85时,所得DGEBHF/BACY胶黏剂的性能最优,此时,Dk=2.95,Df=0.0099,LOI=26.1%;而相同条件下,DGEBA/BACY胶黏剂的Dk=3.04,Df=0.0105,LOI=25.2%。用DOPO-HQ改性BACY,制备得低介电阻燃型氰酸酯胶黏剂。通过GT、DSC和FT-IR表征了DOPO-HQ/BACY胶黏剂的固化性能,结果发现,DOPO-HQ能明显地降低氰酸酯胶黏剂的固化温度和固化时间。通过DEA发现,DOPO-HQ能有效地改善BACY胶黏剂的介电性能,当DOPO-HQ/BACY=10/90时Dk=2.69,Df=0.007。通过测试LOI和UL-94防火等级测试分析了DOPO-HQ/BACY胶黏剂的阻燃性能,结果发现,当添加体系总质量5%的DOPO-HQ后,胶黏剂固化物的LOI=29.7%、UL-94可以达到V-1级,当DOPO-HQ的添加量为10%时,胶黏剂固化物的LOI=33.1%、UL-94可达V-0级。最后,详细地研究了DOPO-HQ/BACY胶黏剂的力学性能和热性能。
[Abstract]:Cyanate resin (CEC) has excellent dielectric properties, high adhesive properties, excellent flame retardancy, high heat resistance, thermal stability and other excellent properties. Ce has become the matrix resin material in many cutting-edge fields (such as aerospace materials, electronic information materials and electrical insulating materials), but the self-catalytic curing temperature of CE is high and the curing time is long. However, many electronic components can not bear the curing temperature and curing time, in addition, the unreacted -OCN in the polycyanate will seriously affect its dielectric properties. At the same time, the flame retardant properties of common cyanate esters can not meet the requirements of the increasing flame retardant properties of modern materials. Therefore, in recent years, the preparation of good curing properties. Cyanate adhesives with excellent dielectric properties and excellent flame retardancy have attracted the attention of many researchers. In this paper, bisphenol A (BPAF) was used. Bisphenol A F epoxy resin (DGEBHF) and 10-C 2. The modified bisphenol A cyanoate (BACYL) was modified by 5-dihydroxyphenyl-10-hydroxy-9-oxa-oxa-10-phenanthroline oxide (DOPO-HQ). Low dielectric flame-retardant cyanate ester adhesives were prepared and their properties were studied in detail. The curing properties of BPAF/BACY adhesives were analyzed by means of gel time, differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR). BPAF can significantly improve the curing properties of BACY. / BPAF / BACY adhesive contrast found that the w BPAF / BACY adhesive has better performance. The effect of the amount of BPAF on the properties of BPAF/BACY adhesive was studied in detail. The results showed that the optimum addition amount of BPAF was 15% of the total mass of the system. The dielectric constant of BPAF/BACY adhesive is 2.68 and the tangent value of dielectric loss angle is 0.0081. The limit oxygen index (loi) is 35.8. the DGEBHF modified BACYs to prepare low dielectric and high toughness cyanate ester adhesive. The properties of bisphenol A epoxy resin DGEBA / BACY adhesive were studied by using GT. The effect of DGEBHF on the curing properties of BACY adhesive was analyzed by DSC and FT-IR. DGEBHF can effectively improve the curing properties of BACY adhesives. The curing properties of BACY adhesives can be analyzed by the addition of the same proportion of epoxy resin. The properties of DGEBHF/BACY adhesive were better than that of DGEBA/BACY adhesive. When DGEBHF/BACY=15/85 was used, the properties of the obtained DGEBHF/BACY adhesive were the best, and the DKN was 2.95% Df0. 0099. Loi 26.1; Under the same conditions, DGEBA / BACY adhesive DKK 3.04% Df0.0105 loi 25.2.The BACY was modified with DOPO-HQ. The low dielectric flame-retardant cyanate ester adhesive was prepared. The curing properties of DOPO-HQ/BACY adhesive were characterized by DOPO-HQ/BACY and FT-IR. DOPO-HQ can obviously reduce the curing temperature and curing time of cyanate ester adhesive. It is found by DEA that DOPO-HQ can effectively improve the dielectric properties of BACY adhesive. Dk=2.69 when DOPO-HQ/BACY=10/90. The flame retardancy of DOPO-HQ/BACY adhesive was analyzed by testing the fire resistance grade of LOI and UL-94. The results showed that the flame retardancy of DOPO-HQ/BACY adhesive was better than that of DOPO-HQ/BACY adhesive. When the total mass of DOPO-HQ was 5%, the content of loi _ (29. 7) and UL-94 of the cementing agent could reach V ~ (-1), and when the amount of DOPO-HQ was 10, the content of the adhesive could reach the level of V ~ (-1). The LOI33.1 / UL-94 adhesives can reach V-0 grade. Finally, the mechanical and thermal properties of DOPO-HQ/BACY adhesives are studied in detail.
【学位授予单位】：西南科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ433.43

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