CdSe量子点发光性质调控和高效胶体量子点发光二极管制备
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摘要
半导体量子点具有尺寸可调谐的光电子性质,已经被广泛地应用于发光二极管、太阳能电池和生物荧光标记。量子点合成技术经过二十多年的发展,人们已经可以合成各种高质量的纳米材料,其光致发光效率可以达到85%以上。由于量子点具有尺寸可调谐的发光、发光线宽窄、光致发光效率高和热稳定性等特点,因此以量子点作为发光层的量子点发光二极管(QD-LED)是极具潜力的下一代显示和固态照明光源。经过科研人员的努力,基于核/壳量子点的QD-LED性能得到了很大的提高,其外量子效率(EQE)从0.001%提高到7%,已经接近于有机发光二极管(OLED)的外量子效率。然而,核/壳量子点中的光物理过程和QD-LED的电致发光机理尚不清楚。因此,研究壳层结构对于量子点光致发光和电致发光性质的影响,对于优化QD-LED器件性能具有重要的意义。本论文主要研究了量子点壳层结构对于其变温发光性质、能量传递过程和电致发光性能的调控,取得的主要研究成果如下:
1、研究了CdSe(核)CdS/ZnCdS/ZnS(多壳层)结构量子点从80 K到360 K的变温发光性质,理解了其辐射与无辐射弛豫过程在这个温度区间内的变化。随着CdSe量子点壳层结构的变化,其温度相关的无辐射过程从热激活的载流子被表面缺陷俘获演变为多个纵光学(LO)声子辅助的热逃逸过程。在包覆厚的CdS壳层和CdS/ZnCdS/ZnS多壳层结构的量子点中,发现光致发光强度随着温度的升高而升高,归因于CdSe/CdS界面局域载流子的热激活过程,其热激活能约为30 meV。实验结果表明多壳层结构可以有效的减少由表面或界面缺陷引起的无辐射复合,同时宽带隙的ZnS壳层可以将电子-空穴限制在量子点内,因此其具有高的发光量子效率和稳定性。
2、通过稳态和时间分辨光谱研究了无机/有机混合薄膜中的CdSe核./壳结构量子点与电子传输材料(ETMs),1,3,5-tris(Nphenylbenzimidazol-2,yl) benzene (TPBI)之间的能量传递过程。TPBI的荧光寿命变短和量子点的荧光寿命变长,说明从供体到受体发生了能量传递。当量子点浓度很低的时候,从量子点周围的TPBI分子到量子点的能量传递达到最大,荧光寿命变长也达到最大。通过拟合得到不同壳层结构量子点周围参与能量传递的TPBI分子的激发态寿命,发现TPBI到包覆CdS/ZnCdS/ZnS多壳层量子点的能量传递速率与包覆薄的ZnS壳层的量子点相当,仅略小于包覆CdS壳层的量子点,归因于CdS与ZnCdS壳层的吸收能量与TPBI的发光能量相匹配,有利于能量传递。实验结果表明可以通过壳层的能级结构和厚度来控制有机分子到量子点的能量传递过程。
3、通过稳态和时间分辨光谱研究了无机/有机混合薄膜中的CdSe核/壳结构量子点与空穴传输材料(HTMs),4,4',4''-Tris(carbazol-9- yl)-triphenylamine (TCTA)或N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'- biphenyl)-4,4'-diamin (TPD)之间的能量传递/电荷分离过程。包覆CdS壳层量子点在TCTA或TPD基质中的荧光寿命明显变短,归因于空穴传输材料对空穴的俘获能力,导致了电荷分离。然而CdSe/CdS/ZnCdS/ZnS核/多壳层量子点在空穴传输材料基质中的荧光寿命没有明显变化,说明多壳层结构有效的抑制了由空穴传输材料引起的电荷分离过程。拟合多壳层结构量子点在TCTA薄膜中的荧光衰减曲线得到,周围TCTA分子到量子点的能量传递效率为35.6%。实验结果表明空穴传输材料的能级结构与量子点的壳层结构共同调控了QD/HTMs混合薄膜中的能量传递/电荷分离过程。
4、将单层量子点旋涂在热交联传输层上,制作了基于不同壳层结构量子点的有机/无机复合多层结构QD-LED。发现CdSe/CdS的QD-LED的外量子效率随着电流密度的增加迅速下降,同时其最大亮度也低于CdSe/ZnS的QD-LED。在包覆CdS和CdS/ZnCdS/ZnS壳层量子点的QD-LED中发现电致发光峰位相对于包覆ZnS壳层的量子点有较大的红移,归因于在电场下电子波函数扩散到壳层中。结果表明包覆宽带隙ZnS壳层的量子点有利于防止激子在电场下离化。
Semiconductor quantum dots (QDs) with size-tunable emission properties have been widely applied in light-emitting diodes (LEDs), photovoltaic cells, and biological labels. The photoluminescence (PL) quantum yield (QY) of QDs reaches 85%, after two decades’development of synthesis technology for QDs. QD based quantum dot light emitting diodes (QD-LEDs) have potential to be the next generation solid state lighting source for display and illumination due to its size-tunable emission wavelength, narrow emission full width at half maximum (FWHM), high PL QY and thermal stability. Recently, the performances of QD-LEDs have a great improvement, for example the external quantum efficiency (EQE) of QD-LEDs is increased from 0.001% to 7%, which approaches to that of organic light emitting diodes (OLEDs). However, the photo-physics processes of core/shell QDs and the electroluminescence (EL) mechanism of QD-LEDs are still not well understood. Therefore, the study for the effects of shell structures of core/shell QDs on the PL and EL mechanism is very important to optimize the performances of QD-LEDs. We study the temperature dependent PL properties of core/shell QDs, energy transfer/ charge separation of QD/ETM or HTM blend films and EL properties of the core/shell QDs. The original works are organized as follows:
1. The photoluminescence spectra of CdSe-core CdS/CdZnS/ZnS-multishellquantum dots were studied to understand the radiative and nonradiative relaxationprocesses in the temperature range from 80 to 360 K. The mechanism oftemperature-dependent nonradiative relaxation processes in the CdSe QDs withchanging the shell structures was found to evolve from thermal activation of carriertrapping by surface defects/traps in CdSe core QDs to the multiplelongitudinal-optical (LO) phonon-assisted thermal escape of carriers in the core/shellQDs. An increase in PL intensity with increasing temperature was clearly observed inthe core/shell QDs with a thick CdS monoshell and a CdS/ZnCdS/ZnS multishell. ThePL enhancement was considered to come from delocalization of charge carrierslocalized at the CdSe/CdS interface with the potential depth of 30 meV. Theexperimental results indicated that the improvement of PL quantum efficiency inCdSe-core CdS/CdZnS/ZnS-multishell QDs could be understood in terms of thereduction of nonradiative recombination centers at the interfaces and on the surface ofthe multishell, as well as the confinement of electrons and holes into the QDs by anouter ZnS shell.
2. The steady-state and time-resolved photoluminescence spectroscopy wasused to study the energy transfer between CdSe core/shell quantum dots and1,3,5-tris(N-phenylbenzimidazol-2,yl) benzene (TPBI) in inorganic/organic blendfilms The shortening in PL lifetime of TPBI molecules and the resulting lengtheningin PL lifetime of the QDs demonstrated an efficient energy transfer process fromdonor to acceptor. The slowest PL decays of CdSe core/shell QDs observed in theblend films with low QD concentration were considered to result from the maximumenergy transfer process from the surrounding TPBI molecules of a QD to itself. ThePL decay curves of the core/shell QDs with a CdS, ZnS, and CdS/ZnCdS/ZnS shellswere simulated to obtain the excited state lifetimes of the surrounding TPBImolecules for understanding the effect of the shells on the energy transfer process. Itwas surprisingly found that the obtained energy transfer rate to a QD with a thickCdS/ZnCdS/ZnS multishell from the surrounding TPBI molecules with the maximumcontribution of the energy transfer was almost the same as that to a QD with a thinZnS monoshell and smaller than that to a QD with a CdS monoshell. Theexperimental results indicated the energy level alignment and the structure of shells inCdSe core/shell QDs determined the energy transfer efficiency from TPBI moleculesto the core/shell QDs.
3. The steady-state and time-resolved photoluminescence spectroscopy was used to study the energy transfer/ charge separation processes in quantum dots and hole transporting materials (HTMs), 4,4',4''-Tris(carbazol-9-yl)-triphenylamine (TCTA) or N,N-diphenyl-N,N'- bis(3-methylphenyl)-(1,1'- biphenyl)-4,4'-diamin (TPD) blend films. Due to the hole capture ability of HTMs, the PL lifetime of CdS shell coated QDs embedding in TCTA or TPD matrix was significantly shortened. However, the PL lifetime of CdSe/CdS/ZnCdS/ZnS core/multi-shell QDs was not changed in HTMs matrix, indicating that the multi-shell suppressed the charge separation at QD/HTM interface. Fitting the PL decay profile of core/multi-shell QDs in TCTA with low QD concentration, the energy transfer efficiency from surrounding TCTA molecules to the central QD was obtained to 35.6%. The experimental results indicated the energy levels of HTMs and shell structure of QDs control the energy transfer/ charge separation in QD/HTMs blend films.
4. The colloidal CdSe/CdS, CdSe/ZnS, and CdSe/CdS/CdZnS/ZnS core/shell quantum dots were fabricated in multilayer light-emitting diodes by spin coating a near monolayer of the core/shell QDs on cross-linkable hole transporting layers. It is found that CdSe/CdS QD-LEDs exhibit a faster decrease in EL quantum efficiency (2% at a brightness of 100 cd/m2) with increasing current density and lower maximum brightness than those of CdSe/ZnS QD-LEDs. A more significant redshift and spectral broadening of the EL observed in CdSe core/ shell QDs with a CdS or CdS/CdZnS/ZnS shell than with a ZnS shell indicate that the electron wave function can penetrate into the shell under electric field. The difference in device performance and EL spectra results from conduction band offsets between the CdSe cores and CdS or ZnS shells, suggesting the existence of the exciton ionization in the QD-LEDs.
1、研究了CdSe(核)CdS/ZnCdS/ZnS(多壳层)结构量子点从80 K到360 K的变温发光性质,理解了其辐射与无辐射弛豫过程在这个温度区间内的变化。随着CdSe量子点壳层结构的变化,其温度相关的无辐射过程从热激活的载流子被表面缺陷俘获演变为多个纵光学(LO)声子辅助的热逃逸过程。在包覆厚的CdS壳层和CdS/ZnCdS/ZnS多壳层结构的量子点中,发现光致发光强度随着温度的升高而升高,归因于CdSe/CdS界面局域载流子的热激活过程,其热激活能约为30 meV。实验结果表明多壳层结构可以有效的减少由表面或界面缺陷引起的无辐射复合,同时宽带隙的ZnS壳层可以将电子-空穴限制在量子点内,因此其具有高的发光量子效率和稳定性。
2、通过稳态和时间分辨光谱研究了无机/有机混合薄膜中的CdSe核./壳结构量子点与电子传输材料(ETMs),1,3,5-tris(Nphenylbenzimidazol-2,yl) benzene (TPBI)之间的能量传递过程。TPBI的荧光寿命变短和量子点的荧光寿命变长,说明从供体到受体发生了能量传递。当量子点浓度很低的时候,从量子点周围的TPBI分子到量子点的能量传递达到最大,荧光寿命变长也达到最大。通过拟合得到不同壳层结构量子点周围参与能量传递的TPBI分子的激发态寿命,发现TPBI到包覆CdS/ZnCdS/ZnS多壳层量子点的能量传递速率与包覆薄的ZnS壳层的量子点相当,仅略小于包覆CdS壳层的量子点,归因于CdS与ZnCdS壳层的吸收能量与TPBI的发光能量相匹配,有利于能量传递。实验结果表明可以通过壳层的能级结构和厚度来控制有机分子到量子点的能量传递过程。
3、通过稳态和时间分辨光谱研究了无机/有机混合薄膜中的CdSe核/壳结构量子点与空穴传输材料(HTMs),4,4',4''-Tris(carbazol-9- yl)-triphenylamine (TCTA)或N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'- biphenyl)-4,4'-diamin (TPD)之间的能量传递/电荷分离过程。包覆CdS壳层量子点在TCTA或TPD基质中的荧光寿命明显变短,归因于空穴传输材料对空穴的俘获能力,导致了电荷分离。然而CdSe/CdS/ZnCdS/ZnS核/多壳层量子点在空穴传输材料基质中的荧光寿命没有明显变化,说明多壳层结构有效的抑制了由空穴传输材料引起的电荷分离过程。拟合多壳层结构量子点在TCTA薄膜中的荧光衰减曲线得到,周围TCTA分子到量子点的能量传递效率为35.6%。实验结果表明空穴传输材料的能级结构与量子点的壳层结构共同调控了QD/HTMs混合薄膜中的能量传递/电荷分离过程。
4、将单层量子点旋涂在热交联传输层上,制作了基于不同壳层结构量子点的有机/无机复合多层结构QD-LED。发现CdSe/CdS的QD-LED的外量子效率随着电流密度的增加迅速下降,同时其最大亮度也低于CdSe/ZnS的QD-LED。在包覆CdS和CdS/ZnCdS/ZnS壳层量子点的QD-LED中发现电致发光峰位相对于包覆ZnS壳层的量子点有较大的红移,归因于在电场下电子波函数扩散到壳层中。结果表明包覆宽带隙ZnS壳层的量子点有利于防止激子在电场下离化。
Semiconductor quantum dots (QDs) with size-tunable emission properties have been widely applied in light-emitting diodes (LEDs), photovoltaic cells, and biological labels. The photoluminescence (PL) quantum yield (QY) of QDs reaches 85%, after two decades’development of synthesis technology for QDs. QD based quantum dot light emitting diodes (QD-LEDs) have potential to be the next generation solid state lighting source for display and illumination due to its size-tunable emission wavelength, narrow emission full width at half maximum (FWHM), high PL QY and thermal stability. Recently, the performances of QD-LEDs have a great improvement, for example the external quantum efficiency (EQE) of QD-LEDs is increased from 0.001% to 7%, which approaches to that of organic light emitting diodes (OLEDs). However, the photo-physics processes of core/shell QDs and the electroluminescence (EL) mechanism of QD-LEDs are still not well understood. Therefore, the study for the effects of shell structures of core/shell QDs on the PL and EL mechanism is very important to optimize the performances of QD-LEDs. We study the temperature dependent PL properties of core/shell QDs, energy transfer/ charge separation of QD/ETM or HTM blend films and EL properties of the core/shell QDs. The original works are organized as follows:
1. The photoluminescence spectra of CdSe-core CdS/CdZnS/ZnS-multishellquantum dots were studied to understand the radiative and nonradiative relaxationprocesses in the temperature range from 80 to 360 K. The mechanism oftemperature-dependent nonradiative relaxation processes in the CdSe QDs withchanging the shell structures was found to evolve from thermal activation of carriertrapping by surface defects/traps in CdSe core QDs to the multiplelongitudinal-optical (LO) phonon-assisted thermal escape of carriers in the core/shellQDs. An increase in PL intensity with increasing temperature was clearly observed inthe core/shell QDs with a thick CdS monoshell and a CdS/ZnCdS/ZnS multishell. ThePL enhancement was considered to come from delocalization of charge carrierslocalized at the CdSe/CdS interface with the potential depth of 30 meV. Theexperimental results indicated that the improvement of PL quantum efficiency inCdSe-core CdS/CdZnS/ZnS-multishell QDs could be understood in terms of thereduction of nonradiative recombination centers at the interfaces and on the surface ofthe multishell, as well as the confinement of electrons and holes into the QDs by anouter ZnS shell.
2. The steady-state and time-resolved photoluminescence spectroscopy wasused to study the energy transfer between CdSe core/shell quantum dots and1,3,5-tris(N-phenylbenzimidazol-2,yl) benzene (TPBI) in inorganic/organic blendfilms The shortening in PL lifetime of TPBI molecules and the resulting lengtheningin PL lifetime of the QDs demonstrated an efficient energy transfer process fromdonor to acceptor. The slowest PL decays of CdSe core/shell QDs observed in theblend films with low QD concentration were considered to result from the maximumenergy transfer process from the surrounding TPBI molecules of a QD to itself. ThePL decay curves of the core/shell QDs with a CdS, ZnS, and CdS/ZnCdS/ZnS shellswere simulated to obtain the excited state lifetimes of the surrounding TPBImolecules for understanding the effect of the shells on the energy transfer process. Itwas surprisingly found that the obtained energy transfer rate to a QD with a thickCdS/ZnCdS/ZnS multishell from the surrounding TPBI molecules with the maximumcontribution of the energy transfer was almost the same as that to a QD with a thinZnS monoshell and smaller than that to a QD with a CdS monoshell. Theexperimental results indicated the energy level alignment and the structure of shells inCdSe core/shell QDs determined the energy transfer efficiency from TPBI moleculesto the core/shell QDs.
3. The steady-state and time-resolved photoluminescence spectroscopy was used to study the energy transfer/ charge separation processes in quantum dots and hole transporting materials (HTMs), 4,4',4''-Tris(carbazol-9-yl)-triphenylamine (TCTA) or N,N-diphenyl-N,N'- bis(3-methylphenyl)-(1,1'- biphenyl)-4,4'-diamin (TPD) blend films. Due to the hole capture ability of HTMs, the PL lifetime of CdS shell coated QDs embedding in TCTA or TPD matrix was significantly shortened. However, the PL lifetime of CdSe/CdS/ZnCdS/ZnS core/multi-shell QDs was not changed in HTMs matrix, indicating that the multi-shell suppressed the charge separation at QD/HTM interface. Fitting the PL decay profile of core/multi-shell QDs in TCTA with low QD concentration, the energy transfer efficiency from surrounding TCTA molecules to the central QD was obtained to 35.6%. The experimental results indicated the energy levels of HTMs and shell structure of QDs control the energy transfer/ charge separation in QD/HTMs blend films.
4. The colloidal CdSe/CdS, CdSe/ZnS, and CdSe/CdS/CdZnS/ZnS core/shell quantum dots were fabricated in multilayer light-emitting diodes by spin coating a near monolayer of the core/shell QDs on cross-linkable hole transporting layers. It is found that CdSe/CdS QD-LEDs exhibit a faster decrease in EL quantum efficiency (2% at a brightness of 100 cd/m2) with increasing current density and lower maximum brightness than those of CdSe/ZnS QD-LEDs. A more significant redshift and spectral broadening of the EL observed in CdSe core/ shell QDs with a CdS or CdS/CdZnS/ZnS shell than with a ZnS shell indicate that the electron wave function can penetrate into the shell under electric field. The difference in device performance and EL spectra results from conduction band offsets between the CdSe cores and CdS or ZnS shells, suggesting the existence of the exciton ionization in the QD-LEDs.
引文
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