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纸质出版日期:2008-6-20,
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覃春杨, 刘烽, 彭波, 黄维, 韦玮. 含空间位阻基团的超支化聚芴的合成、表征及稳定性研究[J]. 高分子学报, 2008,(6):537-543.
QIN Chunyang, LIU Feng, PENG Bo, HUANG Wei, WEI Wei. SYNTHESIS,CHARACTERIZATION AND THERMAL STABILITY OF HYPERBRANCHED POLYFLUORENES CONTAINING STERICALLY HINDERED GROUPS[J]. Acta Polymerica Sinica, 2008,(6):537-543.
覃春杨, 刘烽, 彭波, 黄维, 韦玮. 含空间位阻基团的超支化聚芴的合成、表征及稳定性研究[J]. 高分子学报, 2008,(6):537-543. DOI: 10.3724/SP.J.1105.2008.00537.
QIN Chunyang, LIU Feng, PENG Bo, HUANG Wei, WEI Wei. SYNTHESIS,CHARACTERIZATION AND THERMAL STABILITY OF HYPERBRANCHED POLYFLUORENES CONTAINING STERICALLY HINDERED GROUPS[J]. Acta Polymerica Sinica, 2008,(6):537-543. DOI: 10.3724/SP.J.1105.2008.00537.
以1
3
5-间三溴苯和三(4-溴苯基)胺为支化核,引入9
10-二溴蒽和2
7-二溴-螺(芴-9
9-氧杂蒽) 通过Suzuki反应与芴分别共聚,得到4种不同结构的超支化聚芴蓝光材料,对其结构及光物理性质进行了表征,根据退火前后荧光光谱的变化对其光谱热稳定性进行了研究.实验结果表明,引入超支化结构和高位阻基团,聚芴的荧光发射光谱热稳定性显著提高,绿光区发射现象几乎完全被抑制.
Four kinds of sterically hindered groups-based hyperbranched polyfluorene copolymers containing different branching units such as benzene or triphenylamine were designed and synthesized. All the monomers such as 2
7-dibromo-9
9-dioctylfluorene
2
7-dibromospiro(fluorine-9
9′-xanthene)
9
9-dioctylfluorene-2
7-bis(4
4
5
5-tetramethyl-1
3
2-dioxaborolane) and 9
9-dioctylfluorene-2-boronic acid were prepared according to the literature procedures.Suzuki polycondensation (SPC) with the branching units and linear units was conducted in biphasic system (toluene/aqueous Na2CO3) with Pd(PPh3)4 as a catalyst precursor. The reaction mixture containing monomers was kept stirring at 72℃ under nitrogen for 60 h at the polymerization stage. Then
the end-capped group was added to the reaction mixture together with additional Pd(PPh3) 4 in order to reduce the heavy atom effect which quenched fluorescence. The reaction was continued for further 12 h. After cooling to room temperature
some amount of thiourea was added
and then the mixture was vigorously stirred for another 3 h. The mixture was filtrated to remove the catalyst residues and extracted with toluene. After removal most of the solvent
the crude polymer in certain amount of toluene was added dropwise to methanol and the formed precipitate was recovered by filtration. The solid was washed with methanol
water and again with methanol
then followed by Soxhlet extraction with acetone for 48 h to remove oligomer. The yellow powder was collected and dried under vacuum. All the resulting hyperbranched copolymers are soluble in common organic solvents
such as tetrahydrofuran
chloroform and toluene. The structures of the hyperbranched polymers were fully characterized by NMR
GPC
elementary analysis and thermogravimetric analysis. The degrees of branching of the polymers were calculated through the integration of the characteristic signals of the branching units and linear units from the high-resolution NMR spectroscopy. The GPC experimental results showed that the number-average molecular weights of the polymers were from 11200 to 17200The thermal degradation temperatures (weight loss 5%) of the polymers were nearly at 400℃.Cyclic voltammetry (CV) was used to assess the electrochemical behavior of the polymers. The polymers show a reversible oxidation/reduction wave which can be assigned to the oxidation/reduction potential of copolymer main chain from the onset. The HOMO level of the polymer containing triphenylamine is lower than that containing benzene
which indicated less difficulty in hole injection.The photophysical characteristics of the polymers were investigated in solution and in solid films.Solid films on quartz plates used for UV-Vis
fluorescence were prepared by spin-coating with 10-3 mol/L tetrahydrofuran solution. The absorption maxima of the polymers are blue-shifted within 10 nm compared to that in solution. In addition
the PL maxima remain unchanged or are only slightly red-shifted. Their thermal stability was investigated from the change of fluorescent spectra in solid films after annealing at elevated temperature in air. There was no obvious change in the PL spectra
and no additional green-blue band emission was observed even after the film was annealed at 200℃ in air. Apparently
with the introduction of spirofluorene/large aromatic units to the hyperbranched structure
the red-shifted phenomena and the undesirable low-energy long wavelength emission band are reduced remarkably. All results indicated that the tendency to form aggregate/excimers in the solid state was efficiently suppressed
and the spectral stability of the polymers was greatly improved.
超支化聚芴空间位阻聚集态绿光发射
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