嵌段聚酰亚胺薄膜与荧光性聚酰亚胺—纳米粒子复合薄膜的制备与表征
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摘要
本论文工作介绍了嵌段聚酰亚胺薄膜与荧光性聚酰亚胺-纳米粒子复合薄膜的制备与表征.芳香性聚酰亚作为一种重要的聚合物材料具有优异的综合性能,包括较高的玻璃化转变温度,耐化学腐蚀和耐辐射特性,较低的介电常数和优异的机械性能.由于这些优异的特性聚酰亚胺已经在高性能材料与复合材料领域得到了广泛的应用.芳香性聚酰亚胺较为广泛的应用包括微电子,光电子,汽车,空间工程,先进纺织品和膜技术等领域.近年来的研究趋势是开发能够同时满足多重应用需求的多功能聚酰亚胺材料.
在本论文的第一部分,以刚性较强的二胺单体2-(4-氨基苯基)-5-氨基苯并咪唑(APBI),含有柔性基团醚键的二胺单体4,4’-二氨基二苯醚(ODA)和3,3’,4,4’-联苯四甲酸酐合成(s-BPDA)为聚合原料,合成了一系列的嵌段和无归共聚聚酰亚胺薄膜并对其进行表征.在嵌段共聚物中,刚性棒状的芳杂环二胺APBI形成刚性的链段,而含有醚键的ODA形成了柔性较高的链段.通过调节嵌段长度和刚性／柔性嵌段的含量,制备了六种嵌段聚酰亚胺薄膜.通过控制嵌段长度和嵌段含量,将嵌段聚合物薄膜的热性能与机械性能进行优化.在嵌段聚酰亚胺的制备上,分别合成酸酐基团封端的聚酰胺酸预聚体和氨基封端的聚酰胺酸预聚体,再将二者混合反应以得到长链高分子.APBI在共聚聚酰亚胺中的摩尔含量在10%-60%.聚酰胺酸经过涂膜和高温下热亚胺化的过程得到聚酰亚胺薄膜.为进行对比,合成了与嵌段聚酰亚胺成分相同的无归共聚聚酰亚胺和均聚聚酰亚胺.对制备得到的聚酰亚胺薄膜进行热机械分析(TMA),动态机械分析(DMA),热重分析(TGA),时差扫描量热分析(DSC),广角X-光衍射分析(WAXD),红外分析(FTIR),拉伸测试,吸水率测试和介电常数的测试,以此评估聚合物的热性能,机械性能和电性能.具有分子间氢键键合能力的刚性杂环二胺APBI的引入,可以使聚酰亚胺具有低的热膨胀系数(CTE),较高的玻璃化转变温度,优异的耐热性和机械性能.同时,嵌段共聚聚酰亚胺相比于无归共聚聚酰亚胺具有更好的热性能和机械性能.含APBI60%mol的嵌段共聚聚酰亚胺具有较优异的综合性能,包括低达4.7ppm/K的CTE值,377℃的玻璃化转变温度(Tg),562℃的5%热失重温度(Td5)和198MPa的拉伸强度.这是由于嵌段共聚物中较高的分子链取向导致的,尤其是其较低的CTE值是嵌段聚合物中的局部有序微区导致的.这些局部有序微区并不是结晶的相结构,而是APBI链段参与形成的高度取向和有序的结构.随着APBI链段长度的增加,有序结构的尺寸会随之而增加.与无归共聚聚酰亚胺相比,嵌段共聚物中的高度取向和有序的结构会显著的提高分子链的取向程度.苯并咪唑基团较高的刚性和耐热性导致共聚聚酰亚胺具有更好的热稳定性.TGA分析表明嵌段聚酰亚胺与无归共聚聚酰亚胺相比有更高的Tσ5.这可能是因为刚性APBI链段的形成有助于分子链的堆砌,进而使其耐热性更好.共聚物的Tg随着APBI链段的增长和含量的增加而提高.向聚酰亚胺主链中引入APBI的成分会增加分子链的刚性进而提高分子链段运动的能量势垒,使得Tg得以提高.聚合物机械性能测试结果表明薄膜的拉伸强度和模量随着APBI摩尔含量的增加而增加APBI成分的存在会明显提升聚合物的机械性能.另外,聚苯并咪唑类聚合物(PBIs)由于Π电子的大范围离域而具有良好的机械性能.APBI成分较高的共聚聚酰亚胺薄膜具有稍高的吸水率,这是由于亲水性的咪唑N-H成分更高导致的.共聚聚酰亚胺的介电常数为2.67-3.05,与传统的聚酰亚胺相比较低,但是高于含氟和含有纳米孔的聚酰亚胺.总体来讲,我们所合成的嵌段聚酰亚胺与无归聚酰亚胺相比具有更好的热性能,机械性能和电性能.基于APBI的嵌段聚酰亚胺薄膜作为微电子工业中的基材薄膜具有很大的潜在应用价值.
在论文的第二部分,制备合成了荧光性CdS量子点-聚酰亚胺纳米复合薄膜.在水溶液中合成了高质量的荧光CdS量子点并将其掺杂至聚合物基体中.通常,量子点都是在有机溶剂中合成的.但是,由于有机溶剂法涉及到有毒性的金属有机物的降解,因而方法复杂并并环境有害.所以,在本论文的研究中,我们在水相中制备了CdS量子点,这一方法相对于有机溶剂法更加简便和环境友好.这种方法是在水溶液中直接合成了高质量的水溶性荧光量子点.据此,同时在水相中合成的聚酰亚胺的前驱体,即聚酰胺酸盐,进而制备聚酰亚胺.相比之下,传统的经由聚酰胺酸制备聚酰亚胺的方法有固有的缺陷,比如有机溶剂的使用对环境污染,亚胺化需要高温,聚酰胺酸前驱体的水解稳定性很差.为了避免这些缺陷,我们使用了水相合成的方法.选择水相合成聚合物的另一个重要原因是便于将水溶性的CdS量子点掺杂到聚合物基体中.实验结果表明,CdS量子点均匀的分散与聚酰胺酸盐中.CdS量子点的性能使用XRD,荧光光谱和紫外-可见光谱进行表征.CdS量子点的尺寸为3-5纳米,其具有很好的稳定性和较好的荧光效果.再将水溶性的CdS量子点分散在聚合物基体,即聚酰胺酸盐中.使用PMDA/ODA作为构成聚合物主链的单体,通过添加三乙胺将聚酰胺酸转变为聚酰胺酸盐.将聚酰胺酸盐在丙酮中析出并在真空下烘干,干燥后的粉末可以在水中溶解.纳米复合薄膜通过溶液铺膜和300℃亚胺化制得.使用荧光光谱,XRD,TEM,热机械分析对复合薄膜进行表征.荧光光谱结果表明复合薄膜具有荧光性,相对于CdS量子点水溶液,复合薄膜的光谱有轻微的蓝移和更宽的发射峰.这可能是由聚合物基体的存在和残余的有机溶剂导致的.TEM结果显示CdS量子点均匀分散在薄膜中,尺寸为3-5nm.WAXD结果也证明聚合物基体为无定形状态,而CdS量子点有结晶峰.对纳米复合薄膜的机械性能和热性能进行表征的结果表明CdS能影响材料的热性能和机械性能.随着CdS量子点含量的增加,玻璃化温度有所提高,热稳定性也得到提升.这一现象与无机物填充的聚合物复合材料的性能是相似的.这部分的工作表明,我们成功制备了荧光性CdS量子点／聚酰亚胺纳米复合薄膜.该复合薄膜具有良好的热性能.这种在水相中制备CdS量子点和聚酰亚胺前驱体,进而制备CdS／聚酰亚胺复合薄膜的独特方法可以在光电设备中得到应用.
This dissertation describes the synthesis and characterization of the block copolyimide films and nanocomposite photoluminescent polyimide films. Aromatic polyimides are an important class of polymers used extensively in a variety of high performance materials and composites because of their outstanding physical properties considerably high glass transition temperatures, high resistance to chemicals and radiations, comparatively low dielectric constants, and superior mechanical properties. Some wide-ranging applications of aromatic polyimides include microelectronics, optoelectronics, automotive, aerospace engineering, advance textiles, and membranes technology. The recent trend is the development of multifunctional aromatic polyimides that will attain all desired application-dependent properties simultaneously.
In the first part of this thesis, synthesis and characterization of a series of block and random copolyimide films synthesized from various molar ratios of two diamines, rigid2-(4-Aminophenyl)-5-aminobenzimidazole (APBI) and flexible4,4'-oxydianiline (ODA) by polycondensation with dianhydride3,3',4,4'-biphenyltetracarboxylic dianhydride (sBPDA), is reported. Rigid rod-like heterocyclic diamine APBI diamines produced to rigid blocks while flexible diamine ODA gave rise to relatively flexible segments in block copolyimides. Six block copolyimide films were prepared with systematic variation of block length and block contents of both rigid (APBI-sBPDA) and semi-flexible (ODA-sBPDA) blocks. Thermal and mechanical strength properties of block copolyimides were optimized by controlling block length and contents. Dianhydride-terminated poly(amic acid) oligomer and diamine-terminated poly(amic acid) oligomer were prepared separately and then combined together. The contents of APBI ranged from10to60mol%in copolyimides, Then polymer films were obtained by conventional solution casting method after thermal imidization at elevated temperatures. For comparison purpose, random copolyimides and homopolyimide were also prepared with monomer compositions corresponding to block copolyimides. The copolyimide films obtained by thermal imidization of poly(amic acid)(PAA) solutions, were characterized by-TMA, DMA, TGA, DSC, WAXD. FTIR. tensile testing, water uptake, and dielectric constant measurements, to evaluate their thermal, mechanical strength and electrical properties in details. Rigid heterocyclic diamine APBI with interchain hydrogen bonding capability, led to low CTE, high Tg. high thermal stability and better mechanical properties. Increasing the APBI mol%caused a gradual decrease in the CTE and increase in Tg, thermal stability and tensile strength properties of the copolyimides films. Moreover, significantly enhanced thermal and mechanical properties of the block copolyimides were also found as compared to random copolyimides. The block copolyimide with APBI content of60mol%, achieved excellent properties, i.e., a low CTE (4.7ppm/K), a high Tg at377℃,5%weight loss at562℃and a tensile strength at198MPa. This can be interpreted because of comparatively higher degree of molecular orientation in block copolyimides. The remarkably low CTE values of block copolyimides can be explained in terms of locally ordered microdomains in block copolyimides. These microdomains are not related to crystalline structure but based on highly oriented and well-ordered regions formed by rigid APBI blocks. Microdomains order increases with block length and become more random as block length decreases. The highly oriented and well-ordered block copolyimide structure efficiently promoted molecular orientation in block copolyimides as compared to random copolyimides. The combined effect of heat resistant benzimidazole units and high rigidity led to better thermal stability of copolyimides. TGA analysis indicates that block copolyimides showed slightly higher Tg5than corresponding random copolyimides. This may be due to rigid APBI segments formation, leading to better packing and therefore to higher thermal stability. Tg increased with increasing the rigid APBI block length and molar ratio. Addition of APBI would increase the chain rigidity and therefore increased the potential barrier to rotation, which would result in higher Tg values. Mechanical properties results indicate that tensile strength and tensile modulus increased linearly with increase in APBI mol%. APBI based rigid polymer structure plays a major role in the improvement of mechanical properties. Extensive delocalization of π electrons in PBIs is also well known for their outstanding mechanical properties. Water uptake in copolyimides with higher APBI contents exhibited slightly higher water absorption. This can be attributed to higher concentration of hydrophilic imidazole N-H. Dielectric constants of copolyimides range from2.67to3.05and relatively lower than those of conventional polyimides, but somewhat higher as compared to fluorinated and nanoporous polyimides having ultra-low dielectric constants. Overall, block copolyimides demonstrated better thermal, mechanical and electric properties as compared to simple random copolyimides. APBI based block copolyimide systems can be promising candidates for base film materials in microelectronics applications.
In the second part of dissertation, photoluminescent CdS quantum dots/polyimide nanocomposite films are reported. High quality luminescent CdS quantum dots were synthesized in aqueous medium and then incorporated in polymer matrix. Generally, quantum dots are prepared in organic solvents. However, the organic solvent method is complicated and unsafe to the environment due to the pyrolysis of lethal organometallic reagents. Therefore, in our studies, we prepared water based CdS quantum dots which are simpler to prepare and safer as compared to quantum dots prepared in organic solvents. This procedure includes direct aqueous synthesis route that is environment friendly and produced high quality luminescent water-soluble quantum dots. Accordingly, polyimides were also prepared from water soluble precursor i.e., poly(amic acid) salt rather than conventional poly(amic acid). Conventional preparation technique of polyimides via poly(amic acid) precursor possess some drawbacks, such as, serious damage to the environment because of the toxic volatile polar solvents, elevated thermal imidization temperature and weak hydrolytic stability of poly(amic acid) precursors. To deal with these shortcomings, we selected the water soluble precursor i.e., poly(amic acid) salt. Another major reason was the better incorporation of the water soluble CdS quantum dots in polymer matrix. Water soluble CdS quantum dots were very well dispersed in the poly(amic acid) salt. CdS quantum dots were characterized by XRD, photoluminescence and ultraviolet-visible spectroscopic techniques. Characterization results confirmed the successful synthesis of stable and high quality photoluminescent CdS quantum dots of3-5nm. Next step was the dispersion of water soluble CdS in the polymer matrix. As stated earlier, poly (amic acid) salt precursor was selected for this purpose. Poly (amic acid) was prepared from PMDA/ODA and converted into poly(amic acid) salt by addition of triethylamine. Poly(amic acid) salt solution was precipitated into acetone and vacuum dried. Dried powder was thoroughly dissolved in water. CdS quantum dots solution were mixed with poly(amic acid) salt solution. Nanocomposites films were prepared by solution casting and thermally imidized at300℃. Nanocomposites films were characterized by photoluminescence (PL) measurements, XRD. TEM, Thermomechanical analysis. PL spectra of films showed that nanocomposite films are photoluminescent. PL spectra indicate that there is minor hypsochromic shift and PL peaks are broad as compared to that of pure CdS quantum dots solution. This might be due to the effect of the polymer matrix and presence of organic solvent traces which shift the PL spectra into blue region. TEM micrographs clearly show the presence very well dispersed CdS nanocrystals in films with size of3-5nm. WAXD studies also evidenced the amorphous nature of polyimide films and characteristics CdS nanocrystals peaks. Nanocomposite films were also characterized to evaluate their thermal and mechanical properties. Incorporation of CdS did disturb the mechanical strength and thermal properties. A small rise in glass transition temperature was observed with higher CdS contents. Thermal stability was also enhanced. This phenomenon is common when inorganics were well dispersed in polymer matrix. Results showed that high quality photoluminescent CdS/polyimide nanocomposite films were successfully synthesized. CdS/polyimide nanocomposite films maintained the excellent thermal property of the host polyimide films. This unique approach of preparation of nanocomposite films via water soluble polymer precursor and CdS quantum dots, can find novel applications in electrical and optical devices.
Chapter3reports the synthesis and characterization of six-membered naphthalene dianhydrides based polyimide films and their significantly enhanced thermal and hydrolytic stabilities.4,4'-Binaphthyl-1,1',8,8'-tetracarboxylic dianhydride (BNTDA) and4,4'-Ketone binaphthyl-11',8,8'-tetracarboxylic dianhydride (KBNTDA) were prepared by the dehalogenation-coupling of4-bromo-1,8-naphthalic anhydride and insertion reactions respectively. The structures of BNTDA and KBNTDA were characterized by FTIR,1H-NMR and13C-NMR. A series of polyimides were successfully synthesized from BNTDA, KBNTDA, and various diamines such as4,4'-diaminodiphenyl ether (ODA),4.4'-diaminodiphenylmethane (MDA), and2,5-bis (4-aminophenoxy)-biphenyl (p-TPEQ). The higher molecular weight polyimides exhibited better solubility in common aprotic solvents. The thermal characterization of polyimides by DMA, DSC and TGA techniques, demonstrated super thermal stability of polyimides containing naphthalimide. Glass transition temperature (Tg) of the all polyimides were above326℃and the5%weight loss temperature was above525℃in air and545℃in N2. Hydrolytic stability of the polyimide films was evaluated by immersing the films into deionized water,10%NaOH and10%H2SO4aqueous solutions. Mechanical properties remained stable before and after treatment. Six-membered polyimides derived from KBNTDA and BNTDA, exhibited better hydrolytic stability than those with five-membered phthalic anhydrides.
在本论文的第一部分,以刚性较强的二胺单体2-(4-氨基苯基)-5-氨基苯并咪唑(APBI),含有柔性基团醚键的二胺单体4,4’-二氨基二苯醚(ODA)和3,3’,4,4’-联苯四甲酸酐合成(s-BPDA)为聚合原料,合成了一系列的嵌段和无归共聚聚酰亚胺薄膜并对其进行表征.在嵌段共聚物中,刚性棒状的芳杂环二胺APBI形成刚性的链段,而含有醚键的ODA形成了柔性较高的链段.通过调节嵌段长度和刚性／柔性嵌段的含量,制备了六种嵌段聚酰亚胺薄膜.通过控制嵌段长度和嵌段含量,将嵌段聚合物薄膜的热性能与机械性能进行优化.在嵌段聚酰亚胺的制备上,分别合成酸酐基团封端的聚酰胺酸预聚体和氨基封端的聚酰胺酸预聚体,再将二者混合反应以得到长链高分子.APBI在共聚聚酰亚胺中的摩尔含量在10%-60%.聚酰胺酸经过涂膜和高温下热亚胺化的过程得到聚酰亚胺薄膜.为进行对比,合成了与嵌段聚酰亚胺成分相同的无归共聚聚酰亚胺和均聚聚酰亚胺.对制备得到的聚酰亚胺薄膜进行热机械分析(TMA),动态机械分析(DMA),热重分析(TGA),时差扫描量热分析(DSC),广角X-光衍射分析(WAXD),红外分析(FTIR),拉伸测试,吸水率测试和介电常数的测试,以此评估聚合物的热性能,机械性能和电性能.具有分子间氢键键合能力的刚性杂环二胺APBI的引入,可以使聚酰亚胺具有低的热膨胀系数(CTE),较高的玻璃化转变温度,优异的耐热性和机械性能.同时,嵌段共聚聚酰亚胺相比于无归共聚聚酰亚胺具有更好的热性能和机械性能.含APBI60%mol的嵌段共聚聚酰亚胺具有较优异的综合性能,包括低达4.7ppm/K的CTE值,377℃的玻璃化转变温度(Tg),562℃的5%热失重温度(Td5)和198MPa的拉伸强度.这是由于嵌段共聚物中较高的分子链取向导致的,尤其是其较低的CTE值是嵌段聚合物中的局部有序微区导致的.这些局部有序微区并不是结晶的相结构,而是APBI链段参与形成的高度取向和有序的结构.随着APBI链段长度的增加,有序结构的尺寸会随之而增加.与无归共聚聚酰亚胺相比,嵌段共聚物中的高度取向和有序的结构会显著的提高分子链的取向程度.苯并咪唑基团较高的刚性和耐热性导致共聚聚酰亚胺具有更好的热稳定性.TGA分析表明嵌段聚酰亚胺与无归共聚聚酰亚胺相比有更高的Tσ5.这可能是因为刚性APBI链段的形成有助于分子链的堆砌,进而使其耐热性更好.共聚物的Tg随着APBI链段的增长和含量的增加而提高.向聚酰亚胺主链中引入APBI的成分会增加分子链的刚性进而提高分子链段运动的能量势垒,使得Tg得以提高.聚合物机械性能测试结果表明薄膜的拉伸强度和模量随着APBI摩尔含量的增加而增加APBI成分的存在会明显提升聚合物的机械性能.另外,聚苯并咪唑类聚合物(PBIs)由于Π电子的大范围离域而具有良好的机械性能.APBI成分较高的共聚聚酰亚胺薄膜具有稍高的吸水率,这是由于亲水性的咪唑N-H成分更高导致的.共聚聚酰亚胺的介电常数为2.67-3.05,与传统的聚酰亚胺相比较低,但是高于含氟和含有纳米孔的聚酰亚胺.总体来讲,我们所合成的嵌段聚酰亚胺与无归聚酰亚胺相比具有更好的热性能,机械性能和电性能.基于APBI的嵌段聚酰亚胺薄膜作为微电子工业中的基材薄膜具有很大的潜在应用价值.
在论文的第二部分,制备合成了荧光性CdS量子点-聚酰亚胺纳米复合薄膜.在水溶液中合成了高质量的荧光CdS量子点并将其掺杂至聚合物基体中.通常,量子点都是在有机溶剂中合成的.但是,由于有机溶剂法涉及到有毒性的金属有机物的降解,因而方法复杂并并环境有害.所以,在本论文的研究中,我们在水相中制备了CdS量子点,这一方法相对于有机溶剂法更加简便和环境友好.这种方法是在水溶液中直接合成了高质量的水溶性荧光量子点.据此,同时在水相中合成的聚酰亚胺的前驱体,即聚酰胺酸盐,进而制备聚酰亚胺.相比之下,传统的经由聚酰胺酸制备聚酰亚胺的方法有固有的缺陷,比如有机溶剂的使用对环境污染,亚胺化需要高温,聚酰胺酸前驱体的水解稳定性很差.为了避免这些缺陷,我们使用了水相合成的方法.选择水相合成聚合物的另一个重要原因是便于将水溶性的CdS量子点掺杂到聚合物基体中.实验结果表明,CdS量子点均匀的分散与聚酰胺酸盐中.CdS量子点的性能使用XRD,荧光光谱和紫外-可见光谱进行表征.CdS量子点的尺寸为3-5纳米,其具有很好的稳定性和较好的荧光效果.再将水溶性的CdS量子点分散在聚合物基体,即聚酰胺酸盐中.使用PMDA/ODA作为构成聚合物主链的单体,通过添加三乙胺将聚酰胺酸转变为聚酰胺酸盐.将聚酰胺酸盐在丙酮中析出并在真空下烘干,干燥后的粉末可以在水中溶解.纳米复合薄膜通过溶液铺膜和300℃亚胺化制得.使用荧光光谱,XRD,TEM,热机械分析对复合薄膜进行表征.荧光光谱结果表明复合薄膜具有荧光性,相对于CdS量子点水溶液,复合薄膜的光谱有轻微的蓝移和更宽的发射峰.这可能是由聚合物基体的存在和残余的有机溶剂导致的.TEM结果显示CdS量子点均匀分散在薄膜中,尺寸为3-5nm.WAXD结果也证明聚合物基体为无定形状态,而CdS量子点有结晶峰.对纳米复合薄膜的机械性能和热性能进行表征的结果表明CdS能影响材料的热性能和机械性能.随着CdS量子点含量的增加,玻璃化温度有所提高,热稳定性也得到提升.这一现象与无机物填充的聚合物复合材料的性能是相似的.这部分的工作表明,我们成功制备了荧光性CdS量子点／聚酰亚胺纳米复合薄膜.该复合薄膜具有良好的热性能.这种在水相中制备CdS量子点和聚酰亚胺前驱体,进而制备CdS／聚酰亚胺复合薄膜的独特方法可以在光电设备中得到应用.
This dissertation describes the synthesis and characterization of the block copolyimide films and nanocomposite photoluminescent polyimide films. Aromatic polyimides are an important class of polymers used extensively in a variety of high performance materials and composites because of their outstanding physical properties considerably high glass transition temperatures, high resistance to chemicals and radiations, comparatively low dielectric constants, and superior mechanical properties. Some wide-ranging applications of aromatic polyimides include microelectronics, optoelectronics, automotive, aerospace engineering, advance textiles, and membranes technology. The recent trend is the development of multifunctional aromatic polyimides that will attain all desired application-dependent properties simultaneously.
In the first part of this thesis, synthesis and characterization of a series of block and random copolyimide films synthesized from various molar ratios of two diamines, rigid2-(4-Aminophenyl)-5-aminobenzimidazole (APBI) and flexible4,4'-oxydianiline (ODA) by polycondensation with dianhydride3,3',4,4'-biphenyltetracarboxylic dianhydride (sBPDA), is reported. Rigid rod-like heterocyclic diamine APBI diamines produced to rigid blocks while flexible diamine ODA gave rise to relatively flexible segments in block copolyimides. Six block copolyimide films were prepared with systematic variation of block length and block contents of both rigid (APBI-sBPDA) and semi-flexible (ODA-sBPDA) blocks. Thermal and mechanical strength properties of block copolyimides were optimized by controlling block length and contents. Dianhydride-terminated poly(amic acid) oligomer and diamine-terminated poly(amic acid) oligomer were prepared separately and then combined together. The contents of APBI ranged from10to60mol%in copolyimides, Then polymer films were obtained by conventional solution casting method after thermal imidization at elevated temperatures. For comparison purpose, random copolyimides and homopolyimide were also prepared with monomer compositions corresponding to block copolyimides. The copolyimide films obtained by thermal imidization of poly(amic acid)(PAA) solutions, were characterized by-TMA, DMA, TGA, DSC, WAXD. FTIR. tensile testing, water uptake, and dielectric constant measurements, to evaluate their thermal, mechanical strength and electrical properties in details. Rigid heterocyclic diamine APBI with interchain hydrogen bonding capability, led to low CTE, high Tg. high thermal stability and better mechanical properties. Increasing the APBI mol%caused a gradual decrease in the CTE and increase in Tg, thermal stability and tensile strength properties of the copolyimides films. Moreover, significantly enhanced thermal and mechanical properties of the block copolyimides were also found as compared to random copolyimides. The block copolyimide with APBI content of60mol%, achieved excellent properties, i.e., a low CTE (4.7ppm/K), a high Tg at377℃,5%weight loss at562℃and a tensile strength at198MPa. This can be interpreted because of comparatively higher degree of molecular orientation in block copolyimides. The remarkably low CTE values of block copolyimides can be explained in terms of locally ordered microdomains in block copolyimides. These microdomains are not related to crystalline structure but based on highly oriented and well-ordered regions formed by rigid APBI blocks. Microdomains order increases with block length and become more random as block length decreases. The highly oriented and well-ordered block copolyimide structure efficiently promoted molecular orientation in block copolyimides as compared to random copolyimides. The combined effect of heat resistant benzimidazole units and high rigidity led to better thermal stability of copolyimides. TGA analysis indicates that block copolyimides showed slightly higher Tg5than corresponding random copolyimides. This may be due to rigid APBI segments formation, leading to better packing and therefore to higher thermal stability. Tg increased with increasing the rigid APBI block length and molar ratio. Addition of APBI would increase the chain rigidity and therefore increased the potential barrier to rotation, which would result in higher Tg values. Mechanical properties results indicate that tensile strength and tensile modulus increased linearly with increase in APBI mol%. APBI based rigid polymer structure plays a major role in the improvement of mechanical properties. Extensive delocalization of π electrons in PBIs is also well known for their outstanding mechanical properties. Water uptake in copolyimides with higher APBI contents exhibited slightly higher water absorption. This can be attributed to higher concentration of hydrophilic imidazole N-H. Dielectric constants of copolyimides range from2.67to3.05and relatively lower than those of conventional polyimides, but somewhat higher as compared to fluorinated and nanoporous polyimides having ultra-low dielectric constants. Overall, block copolyimides demonstrated better thermal, mechanical and electric properties as compared to simple random copolyimides. APBI based block copolyimide systems can be promising candidates for base film materials in microelectronics applications.
In the second part of dissertation, photoluminescent CdS quantum dots/polyimide nanocomposite films are reported. High quality luminescent CdS quantum dots were synthesized in aqueous medium and then incorporated in polymer matrix. Generally, quantum dots are prepared in organic solvents. However, the organic solvent method is complicated and unsafe to the environment due to the pyrolysis of lethal organometallic reagents. Therefore, in our studies, we prepared water based CdS quantum dots which are simpler to prepare and safer as compared to quantum dots prepared in organic solvents. This procedure includes direct aqueous synthesis route that is environment friendly and produced high quality luminescent water-soluble quantum dots. Accordingly, polyimides were also prepared from water soluble precursor i.e., poly(amic acid) salt rather than conventional poly(amic acid). Conventional preparation technique of polyimides via poly(amic acid) precursor possess some drawbacks, such as, serious damage to the environment because of the toxic volatile polar solvents, elevated thermal imidization temperature and weak hydrolytic stability of poly(amic acid) precursors. To deal with these shortcomings, we selected the water soluble precursor i.e., poly(amic acid) salt. Another major reason was the better incorporation of the water soluble CdS quantum dots in polymer matrix. Water soluble CdS quantum dots were very well dispersed in the poly(amic acid) salt. CdS quantum dots were characterized by XRD, photoluminescence and ultraviolet-visible spectroscopic techniques. Characterization results confirmed the successful synthesis of stable and high quality photoluminescent CdS quantum dots of3-5nm. Next step was the dispersion of water soluble CdS in the polymer matrix. As stated earlier, poly (amic acid) salt precursor was selected for this purpose. Poly (amic acid) was prepared from PMDA/ODA and converted into poly(amic acid) salt by addition of triethylamine. Poly(amic acid) salt solution was precipitated into acetone and vacuum dried. Dried powder was thoroughly dissolved in water. CdS quantum dots solution were mixed with poly(amic acid) salt solution. Nanocomposites films were prepared by solution casting and thermally imidized at300℃. Nanocomposites films were characterized by photoluminescence (PL) measurements, XRD. TEM, Thermomechanical analysis. PL spectra of films showed that nanocomposite films are photoluminescent. PL spectra indicate that there is minor hypsochromic shift and PL peaks are broad as compared to that of pure CdS quantum dots solution. This might be due to the effect of the polymer matrix and presence of organic solvent traces which shift the PL spectra into blue region. TEM micrographs clearly show the presence very well dispersed CdS nanocrystals in films with size of3-5nm. WAXD studies also evidenced the amorphous nature of polyimide films and characteristics CdS nanocrystals peaks. Nanocomposite films were also characterized to evaluate their thermal and mechanical properties. Incorporation of CdS did disturb the mechanical strength and thermal properties. A small rise in glass transition temperature was observed with higher CdS contents. Thermal stability was also enhanced. This phenomenon is common when inorganics were well dispersed in polymer matrix. Results showed that high quality photoluminescent CdS/polyimide nanocomposite films were successfully synthesized. CdS/polyimide nanocomposite films maintained the excellent thermal property of the host polyimide films. This unique approach of preparation of nanocomposite films via water soluble polymer precursor and CdS quantum dots, can find novel applications in electrical and optical devices.
Chapter3reports the synthesis and characterization of six-membered naphthalene dianhydrides based polyimide films and their significantly enhanced thermal and hydrolytic stabilities.4,4'-Binaphthyl-1,1',8,8'-tetracarboxylic dianhydride (BNTDA) and4,4'-Ketone binaphthyl-11',8,8'-tetracarboxylic dianhydride (KBNTDA) were prepared by the dehalogenation-coupling of4-bromo-1,8-naphthalic anhydride and insertion reactions respectively. The structures of BNTDA and KBNTDA were characterized by FTIR,1H-NMR and13C-NMR. A series of polyimides were successfully synthesized from BNTDA, KBNTDA, and various diamines such as4,4'-diaminodiphenyl ether (ODA),4.4'-diaminodiphenylmethane (MDA), and2,5-bis (4-aminophenoxy)-biphenyl (p-TPEQ). The higher molecular weight polyimides exhibited better solubility in common aprotic solvents. The thermal characterization of polyimides by DMA, DSC and TGA techniques, demonstrated super thermal stability of polyimides containing naphthalimide. Glass transition temperature (Tg) of the all polyimides were above326℃and the5%weight loss temperature was above525℃in air and545℃in N2. Hydrolytic stability of the polyimide films was evaluated by immersing the films into deionized water,10%NaOH and10%H2SO4aqueous solutions. Mechanical properties remained stable before and after treatment. Six-membered polyimides derived from KBNTDA and BNTDA, exhibited better hydrolytic stability than those with five-membered phthalic anhydrides.
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