含硫氟代可自交联聚酰亚胺光波导材料的合成及性能研究
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摘要
本文用设计合成的单体2,2’-二三氟甲基-4,4’-二胺基二苯基硫醚与等摩尔量的二酐单体进行反应。合成的新型聚酰亚胺在通常的溶剂中具有良好的溶解性。它们具有良好的热性能:玻璃化转变温度在221-275℃之间;5%热失重温度在531℃以上。这些含硫氟代聚酰亚胺在加热的情况下可以发生交联反应,交联的机理是硫-硫键交联。交联后的聚合物显示了更加良好的热稳定性;另外这些聚合物交联后在常见的溶剂中不溶解,这也解决了器件加工时的层间互溶问题。聚合物膜具有良好的光学透明性,另外它们在1310nm和1550nm处的光通讯窗口具有较小的吸收。通过控制聚合物中氟原子的含量我们可以控制聚合物的折光指数在1.5626-1.638之间。这些聚合物还具有较小的吸水率,约为0.8%左右。我们还利用所合成的聚合物进行波导器件的制作,制成多种波导器件例如山脊形波导、阵列式波导光栅(AWG)等,由红外摄像机可监测到波导的近场光斑。证明所合成聚合物可用作光波导材料。
The continual trend toward high transmission speed, data capacity, and data density in integrated circuits demands a solution to the bottleneck resulting from the limited data rate of electrical interconnects. One approach to this problem is the use of optical interconnection operating with polymer waveguides. Polymer optical waveguides have attracted considerable attention for their possible application as optical components in optical interconnects and optical communication systems because of their potential ease of manufacture at low temperature, and the low cost of processing.
The key issues on the polymer waveguide materials include four aspects: (1) low propagation losses at the optical communication wavelengths, (2) high thermal stability to provide compatibility with high-performance electronic device fabrication, (3) low birefringence in optical materials is an important issue which can reduce the polarization dependent loss (PDL) (4) controllability of refractive index for the easy control of the waveguide dimension to match the mode size with fibers, and good adhesion to the silicon substrate. However, hydrocarbon polymers have a high optical loss in the infrared communication region due to carbon–hydrogen (C–H) bondvibrational absorption. By modifying a molecule via the substitution of fluorine or deuterium for hydrogen in the C–H greatly reduces optical loss. Many organic polymers such as deuterated or fluorinated poly(methyl methacrylate) (PMMA), polystyrene (PS), and poly(carbonate) (PC) are used as materials for a variety of optical components. However, these polymers do not have sufficient thermal stability at high temperature, for the fabrication temperature of the optical devices is 260 ?C, and the short time temperature is up to 400 ?C. Polyimides are more accessible than these polymers because of their molecular structure. In addition, they have good thermooxidative stability, outstanding mechanical properties, fire resistance and so on. However, conventional polyimide materials possess bad solubility, high moisture adsorption and relatively high dielectric constant, which limit their availability in many field. Many soluble fluorinated polyimides have been synthesized in recent years. Further sul-containing aromatic polymers have great thermal stability for the existence of 3d orbit sulfur atom.
In this study, we introduced the sulfur atom to the famous fluorinated polyimide monomer 2,2’-bis-(trifluoromethyl)-4,4’-diaminobiphenyl (TFDB), and hope the new material can keep the advantage of the famous polyimide. Novel sul-containing fluorinated polyimides have been synthesized by the reaction of 2,2’-bis-(trifluoromethyl)-4,4_-diaminodiphenyl sulfide (TFDAS) with 1,4-bis-(3,4-dicarboxyphenoxy)benzene dianhydride (HQDPA), 2,2’-bis-(3,4-dicarboxyphenyl)hexafluoropropane dianhydride (6FDA), 4,4’-oxydiphthalicanhydride (ODPA) or 3,4,3’,4’-biphenyl-tetracarboxylic acid dianhydride (s-BPDA). The sulfide groups in polymers were introduced to improve adhesion to the Si substrates. The fluorinated polyimides, prepared by a one-step polycondensation procedure, have good solubility in many solvents, such as N-methyl-2-pyrrolidinone (NMP), dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), cyclohexanone, tetrahydrofuran (THF) and m-cresol. The molecular weights (Mn’s) and polydispersities (Mn/Mw’s) of polyimides were in the range of 1.24×105 to 3.21×105 and 1.59–2.20, respectively. The polymers exhibit excellent thermal stabilities, with glass-transition temperatures (Tg) at 221–275 ?C and the 5% weight-loss temperature are above 531 ?C.
The sul-containing fluorinated polyimides can be heated to crosslink. Considering the thermal decomposition, we choose the lower temperature (400 oC) as crosslinking temperature. The probable crosslinking reaction is the reaction between sulfur and sulfur after the polymer cured above a special temperature. After crosslinking, these polymers show higher thermal stability. Furthermore, these polymers are insoluble in common solvent, which can satisfy the need of the interbedded technology of the devices. The sulfide crosslinking will not introduce C–H bond compared to the other common crosslinking groups, thus it can decrease the C–H bond vibrational absorption and lower optical loss will be expected.
The films of polymers have high optical transparency. The novel sul-containing fluorinated polyimides also have low absorption at both 1310 and 1550 nm wavelength windows. The reduction of the refractive indices of the polymers can attribute to the increasing of the fluorine and accretion of the free volume, so it can control the refractive indices of the polymers in the range of 1.5626–1.638 at 1550 nm. They also have a low water absorption rate about 0.8%. TheΔn less than 0.011 was measured in all the polymers. This result is lower (or the same) compared to the conventional fluorinated polyimides. The lowest birefringence of 0.0047 was measured for polyimide 2 film. This may be due to the existence of sulfur atoms and more CF3 groups which decreased the moleculer alignment. Rib-type optical waveguide device was fabricated using the fluorinated polyimides and the near-field mode pattern of the waveguide was demonstrated.
The continual trend toward high transmission speed, data capacity, and data density in integrated circuits demands a solution to the bottleneck resulting from the limited data rate of electrical interconnects. One approach to this problem is the use of optical interconnection operating with polymer waveguides. Polymer optical waveguides have attracted considerable attention for their possible application as optical components in optical interconnects and optical communication systems because of their potential ease of manufacture at low temperature, and the low cost of processing.
The key issues on the polymer waveguide materials include four aspects: (1) low propagation losses at the optical communication wavelengths, (2) high thermal stability to provide compatibility with high-performance electronic device fabrication, (3) low birefringence in optical materials is an important issue which can reduce the polarization dependent loss (PDL) (4) controllability of refractive index for the easy control of the waveguide dimension to match the mode size with fibers, and good adhesion to the silicon substrate. However, hydrocarbon polymers have a high optical loss in the infrared communication region due to carbon–hydrogen (C–H) bondvibrational absorption. By modifying a molecule via the substitution of fluorine or deuterium for hydrogen in the C–H greatly reduces optical loss. Many organic polymers such as deuterated or fluorinated poly(methyl methacrylate) (PMMA), polystyrene (PS), and poly(carbonate) (PC) are used as materials for a variety of optical components. However, these polymers do not have sufficient thermal stability at high temperature, for the fabrication temperature of the optical devices is 260 ?C, and the short time temperature is up to 400 ?C. Polyimides are more accessible than these polymers because of their molecular structure. In addition, they have good thermooxidative stability, outstanding mechanical properties, fire resistance and so on. However, conventional polyimide materials possess bad solubility, high moisture adsorption and relatively high dielectric constant, which limit their availability in many field. Many soluble fluorinated polyimides have been synthesized in recent years. Further sul-containing aromatic polymers have great thermal stability for the existence of 3d orbit sulfur atom.
In this study, we introduced the sulfur atom to the famous fluorinated polyimide monomer 2,2’-bis-(trifluoromethyl)-4,4’-diaminobiphenyl (TFDB), and hope the new material can keep the advantage of the famous polyimide. Novel sul-containing fluorinated polyimides have been synthesized by the reaction of 2,2’-bis-(trifluoromethyl)-4,4_-diaminodiphenyl sulfide (TFDAS) with 1,4-bis-(3,4-dicarboxyphenoxy)benzene dianhydride (HQDPA), 2,2’-bis-(3,4-dicarboxyphenyl)hexafluoropropane dianhydride (6FDA), 4,4’-oxydiphthalicanhydride (ODPA) or 3,4,3’,4’-biphenyl-tetracarboxylic acid dianhydride (s-BPDA). The sulfide groups in polymers were introduced to improve adhesion to the Si substrates. The fluorinated polyimides, prepared by a one-step polycondensation procedure, have good solubility in many solvents, such as N-methyl-2-pyrrolidinone (NMP), dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO), cyclohexanone, tetrahydrofuran (THF) and m-cresol. The molecular weights (Mn’s) and polydispersities (Mn/Mw’s) of polyimides were in the range of 1.24×105 to 3.21×105 and 1.59–2.20, respectively. The polymers exhibit excellent thermal stabilities, with glass-transition temperatures (Tg) at 221–275 ?C and the 5% weight-loss temperature are above 531 ?C.
The sul-containing fluorinated polyimides can be heated to crosslink. Considering the thermal decomposition, we choose the lower temperature (400 oC) as crosslinking temperature. The probable crosslinking reaction is the reaction between sulfur and sulfur after the polymer cured above a special temperature. After crosslinking, these polymers show higher thermal stability. Furthermore, these polymers are insoluble in common solvent, which can satisfy the need of the interbedded technology of the devices. The sulfide crosslinking will not introduce C–H bond compared to the other common crosslinking groups, thus it can decrease the C–H bond vibrational absorption and lower optical loss will be expected.
The films of polymers have high optical transparency. The novel sul-containing fluorinated polyimides also have low absorption at both 1310 and 1550 nm wavelength windows. The reduction of the refractive indices of the polymers can attribute to the increasing of the fluorine and accretion of the free volume, so it can control the refractive indices of the polymers in the range of 1.5626–1.638 at 1550 nm. They also have a low water absorption rate about 0.8%. TheΔn less than 0.011 was measured in all the polymers. This result is lower (or the same) compared to the conventional fluorinated polyimides. The lowest birefringence of 0.0047 was measured for polyimide 2 film. This may be due to the existence of sulfur atoms and more CF3 groups which decreased the moleculer alignment. Rib-type optical waveguide device was fabricated using the fluorinated polyimides and the near-field mode pattern of the waveguide was demonstrated.
引文
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