纳米硫化物修饰的支链含杂原子功能高分子的合成与性能研究
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摘要
聚合物纳米复合物(PNCs)兼具聚合物和纳米粒子的性质,因此具有特殊的力学、热学、摩擦学、光学、发光学、磁学、电学以及催化等性能。本文合成了多种功能高分子及其纳米复合物,包括:(1)侧链巯基功能化聚苯乙烯/CdS(thiol-functional polystyrene/CdS,TPSC);(2)聚苯乙烯-b-聚4-乙烯基吡啶/ML(M=Cd,Zn;L=S,Se)(polystyrene-b-poly(4-vinylpyridine)/ML,PS4VP/ML);(3)聚(N-苯基马来酰亚胺)-b-聚(4-乙烯基吡啶)/ML(M=Cd,Zn;L=S,Se)(PNPMI-b-P4VP/ML);聚(N-苯基马来酰亚胺)-b-聚(N,N-二甲基甲基丙烯酰胺)/ML(M=Cd,Zn;L=S,Se)(poly(N-phenylmaleimide-b-dimethylamino methacrylate)/ML,PNPMI-b-PDMAM/ML);(4)聚(3-烷基噻吩)/MS(M=Cd,Zn )( poly(3-alkylthiophenes)/MS , P3ATs/MS )和聚( 3-烷氧基噻吩)(poly(3-alkoxythiophenes),P3AOTs)等。通过将高分子与纳米半导体的复合,以提高材料的稳定性和光致发光(PL)和三阶非线性光学(NLO)等光学性能。分别采用自由基共聚(RP)和可逆加成-断裂链转移活性自由基聚合(RAFT)的方法控制聚合物和纳米复合物的组成、纳米粒子的粒径及晶型以及复合物的形态结构,以调控材料的光学性质。
1、TPSC聚合物纳米复合物:通过控制投料比有效地调控了侧链巯基功能化聚苯乙烯(thiol-functional polystyrene,TPS)及TPSC的组成、纳米粒子的粒径、晶型以及TPSC的光致发光性质。随着CdS含量的增加,TPSC中CdS的晶型由立方型向六方型转变,TPSC的光致发光主要来自纳米CdS。由于具有量子效应,CdS对TPS的荧光具有增强作用。
2、PS4VP/CdS( ZnS ,CdSe )纳米复合物:首次以4-乙烯基吡啶/M~(2+)(4-vinylpyridine/M~(2+),4VP/M~(2+))为单体,经RAFT和原位生成法制备了PS4VP/CdS等纳米复合物,通过活性聚合有效地调控了纳米复合物的组成以及纳米粒子的粒径和晶型,进而有效地调控了纳米复合物的光致发光性质。随着RAFT聚合时间的增加,复合物中纳米粒子的含量不断提高,粒径增大,复合物趋于聚集、收缩并自组装。通过改变浓度、纳米粒子含量、分散剂等调控了复合物形态,制备出纳米膜、纳米棒、纳米网孔结构以及高规整度的纳米线结构等纳米复合物。纳米复合物的光致发光随着纳米粒子含量的改变由聚合物和纳米粒子的共同发光转变为以纳米粒子的发光为主。通过在纳米复合物中引入ZnS(蓝色)、CdS(黄绿色)、CdSe(橙红色)等不同的纳米粒子,有效地调节了复合物的光致发光性质,得到了发白光的PS4VP/ZnS/CdS/CdSe纳米复合物。
3、PNPMI-b-P4VP/CdS(ZnS,CdSe)、PNPMI-b-PDMAM/ CdS(ZnS,CdSe)纳米复合物:首次以4VP/M~(2+),N,N-二甲基甲基丙烯酰胺/M~(2+)(dimethylamino methacrylate , DMAM/M~(2+) )为单体,经RAFT和原位生成法制备了PNPMI-b-P4VP/CdS(ZnS,CdSe),PNPMI-b-PDMAM/CdS(ZnS,CdSe)等聚合物纳米复合物。通过活性聚合有效地调控了纳米复合物的组成、纳米粒子的粒径和晶型,以及复合物的光致发光和三阶NLO性能。随着RAFT聚合时间的增加,复合物中纳米粒子的含量不断提高,粒径增大,复合物的光致发光由聚合物和纳米粒子的共同发光转变为以纳米粒子的荧光为主。通过在纳米复合物中引入ZnS、CdS、CdSe等不同的纳米粒子,有效地调节了复合物的荧光性质,并得到发白光的PNPMI-b-P4VP/ZnS/CdS/CdSe和PNPMI-b-PDMAM/ZnS/CdS/CdSe等纳米复合物。合成的纳米复合物还具有三阶NLO性能,这是纳米粒子与聚合物之间强烈的相干振荡作用的结果。
4、聚(3-烷基噻吩)(P3ATs)和聚(3-烷氧基噻吩)(P3AOTs)及其纳米复合物:研究了烷基侧链对聚合物规整性、荧光和非线性光学性能的影响,以及纳米复合物的发光机理。研究表明,随着烷基侧链的增大,P3ATs的规整性下降,吸收光谱蓝移,荧光增强,NLO性质和导电性降低。随着纳米粒子含量的提高,复合物的光致发光大多由聚合物发光向纳米粒子发光转变。聚(3-十二烷基噻吩)/CdS(P3DDT/CdS)的激发和发射基本不随CdS含量的改变而变化,这是因为P3DDT/CdS的价带偏移大于导带偏移,电子和空穴在P3DDT中复合发光。复合物的三阶NLO系数高于P3ATs,这是因为纳米粒子与聚合物之间存在强烈的相互作用。
The study of polymer nanocoposites (PNCs) focus on their mechanical, thermal, tribological, optical transparency, luminescence, magnetic, electrical and catalytic properties. In the present work, some functional polymers and their nanocomposites have been prepared, such as thiol-functional polystyrene/CdS (TPSC), polystyrene-b-poly(4-vinylpyridine)/ML (M=Cd, Zn; L=S, Se) (PS4VP/ML), poly(N-phenylmaleimide-b-4-vinylpyridine)/ML(M=Cd,Zn;L=S,Se)(PNPMI-b-P4VP/ML), poly(N-phenylmaleimide-b-dimethylamino methacrylate)/ML(M=Cd, Zn; L=S, Se) (PNPMI-b-PDMAM/ML), poly(3-alkylthiophene)/MS(M=Cd, Zn) (P3ATs/MS) and poly(3-alkoxythiophenes) (P3AOTs). The combination of nanoparticles with polymers can promote the stability and fluorescence yield of materials, also their nonlinear optics performance. The optical properties of PNCs are related to the structure of composites, which determined by the size and dispersion of nanoparticles. To control the composition of polymer, the content and size of nanoparticles, also the structure of PNCs, the radical polymerization (RP) and reversible addition-fragmentation chain transfer (RAFT) methods have been used to synthesize the functional polymers, then the corresponding PNCs were prepared by in-situ method.
1. Synthesis of the TPSC and study on the method to control the content and size of CdS in the composites. The composition of polystyrene-co-polychloromethylstyrene can be determined by the styrene-to-chloromethylstyren ratio during copolymerization, then the thiol content is determined. The CdS concentration is also changed through different thiol-to-CdCl_2 ratio. The crystal styles of CdS in the TPSC are also changed from cubic to hexagonal with increasing CdS content. The PL properties of TPSC are promoted by the CdS nanoparticles, which having quantum effect. The PL mainly comes from CdS.
2. PS4VP/CdS (ZnS, CdSe) have been prepared by RAFT polymerization using 4VP/M~(2+) as monomers for the first time. The composition, molecular weight and their dispersion of polymers are controlled well by living polymerization. The tunable crystal styles of CdS (from cubic to hexagonal) and optical properties of PNCs also have been realized. The nanoparticles tend to congregate together with the increasing polymeric time, resulting in the growth of nanoparticles and the self-assembly of PNCs. The morphology of PNCs are also changed from nanofilms, nanorods, netholes to nanowires by changing the concentration of PNCs, the content of nanoparticles, the environment temperature or the solvent for dispersion of composites. The legend-centered charge-transfer (LCCT) and LMCT mechanism coexist in the PNCs containing a small quantity of nanoparticles. However, the LMCT is the dominant mechanism in the PNCs with a high content of nanoparticles i.e. the LCCT tends to convert to LMCT when the concentration of nanoparticles increases. The photoluminescence properties of PNCs are tuned up by ZnS, CdS and CdSe nanoparticles, and some white light PNCs such as PS4VP/ZnS/CdS/CdSe were obtained.
3. The PNPMI-b-P4VP/CdS(ZnS, CdSe) and PNPMI-b-PDMAM/CdS(ZnS, CdSe) PNCs have been prepared by RAFT polymerization using 4VP/M~(2+) and DMAM/M~(2+) as monomers for the first time. The composition, molecular weight and their dispersion of polymers are controlled well by living polymerization. The obtained PNCs have tunable crystal styles of nanoparticles and optical properties of PNCs. The nanoparticles tend to congregate together with the increasing polymerization time, resulting in the growth of nanoparticles and the self-assembly of PNCs. The morphology of PNCs are also varied by changing the concentration of PNCs, the content of nanoparticles, the environment temperature or the solvent for dispersion of composites. The ligand-centered charge-transfer (LCCT) and LMCT mechanism coexist in the PNCs containing a small quantity of nanoparticles. However, the LMCT is the dominant mechanism in the PNCs with a high content of nanoparticles i.e. the LCCT tends to convert to LMCT when the concentration of nanoparticles increases. The photoluminescence (PL) properties of PNCs are tuned up by ZnS, CdS and CdSe nanoparticles, and some white light PNCs such as PNPMI-b-P4VP/ZnS/CdS/CdSe and PNPMI-b-PDMAM/ZnS/CdS/CdSe were obtained. The NLO absorption and refraction of PNCs are also strong, resulting from the interaction between the nanoparticles and the polymers.
4. P3ATs and P3AOTs were synthesized by chemical oxidation and the P3ATs/MS(M=Cd, Zn) were prepared by in-situ method. The effect of alkyl sidechains on the regioregularity and the optical properties of P3ATs were studied, respectively. The dependence of PL and NLO properties of PNCs on the nanoparticles also introduced. The ratio of head-to-tail (HT) coupling in the P3ATs decreases with the carbon number of sidechains increasing from 3 to 12, combing with a blue shift of absorption and a stronger PL intensity. The NLO properties and conductivity of P3ATs with a larger alkyl group decrease. The LMCT and LCCT coexist in the P3ATs/MS, and also are changeable. Interestingly, the excited wavelength and emission peaks of poly(3-dodecyl thiophene)/CdS (P3DDT/CdS) could not be changed by changing the CdS content. This is assigned to the valence band offset is larger than their conduction band offset, so, the electron-hole recombination mainly occurred in the P3DDT. The NLO performance of P3ATs/MS are better than that of P3ATs. The surface-induced charge separation (i.e. the coherent oscillation of the conduction band electrons) is expected to enhance the anisotropic polarization and hence the nonlinear optical response.
1、TPSC聚合物纳米复合物:通过控制投料比有效地调控了侧链巯基功能化聚苯乙烯(thiol-functional polystyrene,TPS)及TPSC的组成、纳米粒子的粒径、晶型以及TPSC的光致发光性质。随着CdS含量的增加,TPSC中CdS的晶型由立方型向六方型转变,TPSC的光致发光主要来自纳米CdS。由于具有量子效应,CdS对TPS的荧光具有增强作用。
2、PS4VP/CdS( ZnS ,CdSe )纳米复合物:首次以4-乙烯基吡啶/M~(2+)(4-vinylpyridine/M~(2+),4VP/M~(2+))为单体,经RAFT和原位生成法制备了PS4VP/CdS等纳米复合物,通过活性聚合有效地调控了纳米复合物的组成以及纳米粒子的粒径和晶型,进而有效地调控了纳米复合物的光致发光性质。随着RAFT聚合时间的增加,复合物中纳米粒子的含量不断提高,粒径增大,复合物趋于聚集、收缩并自组装。通过改变浓度、纳米粒子含量、分散剂等调控了复合物形态,制备出纳米膜、纳米棒、纳米网孔结构以及高规整度的纳米线结构等纳米复合物。纳米复合物的光致发光随着纳米粒子含量的改变由聚合物和纳米粒子的共同发光转变为以纳米粒子的发光为主。通过在纳米复合物中引入ZnS(蓝色)、CdS(黄绿色)、CdSe(橙红色)等不同的纳米粒子,有效地调节了复合物的光致发光性质,得到了发白光的PS4VP/ZnS/CdS/CdSe纳米复合物。
3、PNPMI-b-P4VP/CdS(ZnS,CdSe)、PNPMI-b-PDMAM/ CdS(ZnS,CdSe)纳米复合物:首次以4VP/M~(2+),N,N-二甲基甲基丙烯酰胺/M~(2+)(dimethylamino methacrylate , DMAM/M~(2+) )为单体,经RAFT和原位生成法制备了PNPMI-b-P4VP/CdS(ZnS,CdSe),PNPMI-b-PDMAM/CdS(ZnS,CdSe)等聚合物纳米复合物。通过活性聚合有效地调控了纳米复合物的组成、纳米粒子的粒径和晶型,以及复合物的光致发光和三阶NLO性能。随着RAFT聚合时间的增加,复合物中纳米粒子的含量不断提高,粒径增大,复合物的光致发光由聚合物和纳米粒子的共同发光转变为以纳米粒子的荧光为主。通过在纳米复合物中引入ZnS、CdS、CdSe等不同的纳米粒子,有效地调节了复合物的荧光性质,并得到发白光的PNPMI-b-P4VP/ZnS/CdS/CdSe和PNPMI-b-PDMAM/ZnS/CdS/CdSe等纳米复合物。合成的纳米复合物还具有三阶NLO性能,这是纳米粒子与聚合物之间强烈的相干振荡作用的结果。
4、聚(3-烷基噻吩)(P3ATs)和聚(3-烷氧基噻吩)(P3AOTs)及其纳米复合物:研究了烷基侧链对聚合物规整性、荧光和非线性光学性能的影响,以及纳米复合物的发光机理。研究表明,随着烷基侧链的增大,P3ATs的规整性下降,吸收光谱蓝移,荧光增强,NLO性质和导电性降低。随着纳米粒子含量的提高,复合物的光致发光大多由聚合物发光向纳米粒子发光转变。聚(3-十二烷基噻吩)/CdS(P3DDT/CdS)的激发和发射基本不随CdS含量的改变而变化,这是因为P3DDT/CdS的价带偏移大于导带偏移,电子和空穴在P3DDT中复合发光。复合物的三阶NLO系数高于P3ATs,这是因为纳米粒子与聚合物之间存在强烈的相互作用。
The study of polymer nanocoposites (PNCs) focus on their mechanical, thermal, tribological, optical transparency, luminescence, magnetic, electrical and catalytic properties. In the present work, some functional polymers and their nanocomposites have been prepared, such as thiol-functional polystyrene/CdS (TPSC), polystyrene-b-poly(4-vinylpyridine)/ML (M=Cd, Zn; L=S, Se) (PS4VP/ML), poly(N-phenylmaleimide-b-4-vinylpyridine)/ML(M=Cd,Zn;L=S,Se)(PNPMI-b-P4VP/ML), poly(N-phenylmaleimide-b-dimethylamino methacrylate)/ML(M=Cd, Zn; L=S, Se) (PNPMI-b-PDMAM/ML), poly(3-alkylthiophene)/MS(M=Cd, Zn) (P3ATs/MS) and poly(3-alkoxythiophenes) (P3AOTs). The combination of nanoparticles with polymers can promote the stability and fluorescence yield of materials, also their nonlinear optics performance. The optical properties of PNCs are related to the structure of composites, which determined by the size and dispersion of nanoparticles. To control the composition of polymer, the content and size of nanoparticles, also the structure of PNCs, the radical polymerization (RP) and reversible addition-fragmentation chain transfer (RAFT) methods have been used to synthesize the functional polymers, then the corresponding PNCs were prepared by in-situ method.
1. Synthesis of the TPSC and study on the method to control the content and size of CdS in the composites. The composition of polystyrene-co-polychloromethylstyrene can be determined by the styrene-to-chloromethylstyren ratio during copolymerization, then the thiol content is determined. The CdS concentration is also changed through different thiol-to-CdCl_2 ratio. The crystal styles of CdS in the TPSC are also changed from cubic to hexagonal with increasing CdS content. The PL properties of TPSC are promoted by the CdS nanoparticles, which having quantum effect. The PL mainly comes from CdS.
2. PS4VP/CdS (ZnS, CdSe) have been prepared by RAFT polymerization using 4VP/M~(2+) as monomers for the first time. The composition, molecular weight and their dispersion of polymers are controlled well by living polymerization. The tunable crystal styles of CdS (from cubic to hexagonal) and optical properties of PNCs also have been realized. The nanoparticles tend to congregate together with the increasing polymeric time, resulting in the growth of nanoparticles and the self-assembly of PNCs. The morphology of PNCs are also changed from nanofilms, nanorods, netholes to nanowires by changing the concentration of PNCs, the content of nanoparticles, the environment temperature or the solvent for dispersion of composites. The legend-centered charge-transfer (LCCT) and LMCT mechanism coexist in the PNCs containing a small quantity of nanoparticles. However, the LMCT is the dominant mechanism in the PNCs with a high content of nanoparticles i.e. the LCCT tends to convert to LMCT when the concentration of nanoparticles increases. The photoluminescence properties of PNCs are tuned up by ZnS, CdS and CdSe nanoparticles, and some white light PNCs such as PS4VP/ZnS/CdS/CdSe were obtained.
3. The PNPMI-b-P4VP/CdS(ZnS, CdSe) and PNPMI-b-PDMAM/CdS(ZnS, CdSe) PNCs have been prepared by RAFT polymerization using 4VP/M~(2+) and DMAM/M~(2+) as monomers for the first time. The composition, molecular weight and their dispersion of polymers are controlled well by living polymerization. The obtained PNCs have tunable crystal styles of nanoparticles and optical properties of PNCs. The nanoparticles tend to congregate together with the increasing polymerization time, resulting in the growth of nanoparticles and the self-assembly of PNCs. The morphology of PNCs are also varied by changing the concentration of PNCs, the content of nanoparticles, the environment temperature or the solvent for dispersion of composites. The ligand-centered charge-transfer (LCCT) and LMCT mechanism coexist in the PNCs containing a small quantity of nanoparticles. However, the LMCT is the dominant mechanism in the PNCs with a high content of nanoparticles i.e. the LCCT tends to convert to LMCT when the concentration of nanoparticles increases. The photoluminescence (PL) properties of PNCs are tuned up by ZnS, CdS and CdSe nanoparticles, and some white light PNCs such as PNPMI-b-P4VP/ZnS/CdS/CdSe and PNPMI-b-PDMAM/ZnS/CdS/CdSe were obtained. The NLO absorption and refraction of PNCs are also strong, resulting from the interaction between the nanoparticles and the polymers.
4. P3ATs and P3AOTs were synthesized by chemical oxidation and the P3ATs/MS(M=Cd, Zn) were prepared by in-situ method. The effect of alkyl sidechains on the regioregularity and the optical properties of P3ATs were studied, respectively. The dependence of PL and NLO properties of PNCs on the nanoparticles also introduced. The ratio of head-to-tail (HT) coupling in the P3ATs decreases with the carbon number of sidechains increasing from 3 to 12, combing with a blue shift of absorption and a stronger PL intensity. The NLO properties and conductivity of P3ATs with a larger alkyl group decrease. The LMCT and LCCT coexist in the P3ATs/MS, and also are changeable. Interestingly, the excited wavelength and emission peaks of poly(3-dodecyl thiophene)/CdS (P3DDT/CdS) could not be changed by changing the CdS content. This is assigned to the valence band offset is larger than their conduction band offset, so, the electron-hole recombination mainly occurred in the P3DDT. The NLO performance of P3ATs/MS are better than that of P3ATs. The surface-induced charge separation (i.e. the coherent oscillation of the conduction band electrons) is expected to enhance the anisotropic polarization and hence the nonlinear optical response.
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