Research Article Cite This: ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
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Stretchable and Ambient Stable Perovskite/Polymer Luminous Hybrid Nanofibers of Multicolor Fiber Mats and Their White LED Applications Ender Ercan,† Ping-Chun Tsai,‡ Jung-Yao Chen,† Jeun-Yen Lam,‡ Li-Che Hsu,‡ Chu-Chen Chueh,†,§ and Wen-Chang Chen*,†,§ Department of Chemical Engineering, ‡Institute of Polymer Science and Engineering, and §Advanced Research Center of Green Materials Science and Technology, National Taiwan University, Taipei 10617, Taiwan
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S Supporting Information *
ABSTRACT: We report the fabrication and optical/mechanical properties of perovskite/thermoplastic polyurethane (TPU)-based multicolor luminescent core−shell nanofibers and their large-scale fiber mats. One-step coaxial perovskite/TPU nanofibers had a high photoluminescence quantum yield value exceeding 23.3%, surpassing that of its uniaxial counterpart, due to the homogeneous distribution of perovskite nanoparticles (NPs) by the confinement of the TPU shell. The fabricated core−shell nanofibers exhibited a high mechanical endurance owing to the well elastic properties of TPU and maintained the luminescence intensity even under a 100% stretched state after 1000 stretching−relaxing cycles. By taking advantage of the hydrophobic nature of TPU, the ambient and moisture stability of the fabricated fibers were enhanced up to 1 month. Besides, large-area stretchable nanofibers with a dimension of 15 cm × 30 cm exhibiting various visible-light emission peaks were fabricated by changing the composition of perovskite NPs. Moreover, a large-scale luminescent and stretchable fiber mat was successfully fabricated by electrospinning. Furthermore, the white-light emission from the fabricated fibers and mats was achieved by incorporating orange-light-emitting poly[2-methoxy-5-(2-ethylhexyloxy)-1,4phenylenevinylene] into the TPU shell and coupling the turquoise blue-light-emitting perovskite NPs in the core site. Finally, the integrity of the perovskite-based TPU fibers was realized by fabricating a light-emitting diode (LED) device containing the orange-light-emitting fibers embedded in the polyfluorene emissive layer. This work demonstrated an effective way to prepare stable and stretchable luminous nanofibers and the integration of such nanofibers into LED devices, which could facilitate the future development of wearable electronic devices. KEYWORDS: perovskite, hybrid, luminescence, nanofibers, stretchable fibers, white LED
1. INTRODUCTION In recent years, stretchable electronics has been considered as the most important next-generation consumer products since they possess decent flexibility, foldability, bendability, and stretchability that can well meet the ergonomic needs. In response to this emerging demand, numerous research efforts have been dedicated and various stretchable optoelectronic devices have been developed, such as light-emitting diodes (LEDs),1−5 solar cells,6−9 field-effect transistors,10,11 memory devices,12−16 etc. The stretchable apparatuses possess a promising potential for the future development of advanced electronics, such as smart phones, wearable electronics, and mobile electronics. To exploit efficient stretchable devices, the engineering at both material and device levels has been widely investigated. From the material aspect, owing to the superior ductility, organic semiconductors have attracted more attention than the inorganic materials that are generally highly crystalline. However, recently, organic−inorganic hybrid perovskites have become a rising star in various optoelectronic fields due © 2019 American Chemical Society
to their tunable band gap and solution-based processability, including memories,17−25 LEDs,26−28 and light-harvesting applications.29−32 The tunable band gap of organic−inorganic hybrid perovskites could be achieved by simply tuning the composition of perovskite materials.33,34 Accompanied by this feature, the concomitant light emission of the materials can be also simply tuned and show a narrow emission range, thus manifesting promising potential for light-emitting applications in addition to the prevailing light-harvesting applications. However, the stretchability of such class of materials remains a significant challenge. Therefore, how to integrate the perovskites into the development of stretchable materials has attracted myriads of research interest in these years. It is worth noting that the dimension of perovskite materials had been proven to have a significant impact on the resultant Received: March 28, 2019 Accepted: June 6, 2019 Published: June 6, 2019 23605
DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
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ACS Applied Materials & Interfaces
nanofibers into light-emitting devices for flexible or wearable electronic devices.
high photoluminescence quantum yield (PLQY) through the whole visible range, similar to the quantum confinement effect observed in the nanodimensional crystals.35 For example, organic−inorganic perovskite nanodots with a high PLQY of 83% were reported by controlling their crystal growth conditions.36 Such impressive result indicates the feasibility of using organic−perovskite hybrids to prepare stretchable luminous materials. It suggests that the luminous perovskite nanoparticles (NPs) can be embedded in a uniform polymer matrix possessing respectable stretchability. Based on this rationale, we herein are interested in developing stretchable, luminous perovskite nanofibers. On the one hand, the perovskite NPs can grow in the polymer template (or matrix) by taking advantage of chemical interactions between them.37−40 On the other hand, the electrospinning technique endows the homogeneous distribution of perovskite NPs through the fabricated nanofibers, as demonstrated in our recent work.41 We successfully fabricated uniform luminous perovskite/polymer electrospun nanofibers using one-step core−shell (or named as coaxial) electrospinning technique and manifested that the perovskite NPs were homogeneously dispersed inside the nanofibers.41 However, achieving stretchable white-light-emitting fibers and the compatibility of nanofibers in LED device to tune the desired emission color remain significant challenges. Standing on this basis, we thus propose to prepare hybrid organic−inorganic-based white-light-emitting stretchable nanofibers using emissive an organic and stretchable polymer as a shell. Moreover, a new approach for the nanofiberintegrated LED device has to be developed on tuning the desired color of emission benefiting from energy transfer. In this study, we report the fabrication and optical/ mechanical properties of perovskite/thermoplastic polyurethane (TPU) based multicolor luminescent core−shell nanofibers and their large-scale fiber mats. The thermoplastic polyurethane (TPU) was employed as the stretchable polymeric shell due to the rubberlike elastic properties. Besides, TPU also possesses a hydrophobic nature and is nontoxic and biocompatible, which are very suitable for integration in the smart textiles.42 We first used the one-step coaxial electrospinning technique to fabricate luminescent electrospun TPU/perovskite nanofibers and compared with the nanofibers prepared by the regular uniaxial electrospinning method. Then, the perovskite nanoparticles were grown inside the fibers and their morphologies were characterized by transmission electron microscopy (TEM). In the following, the physical properties of the prepared core−shell fibers were characterized under the ambient condition, including optical absorption, photoluminescence (PL), and mechanical stretching. By changing the composition of perovskite NPs, stretchable nanofibers with various visible-light emission peaks were fabricated. Furthermore, white-light emission of the fabricated fibers and mats was achieved by incorporating orange-light-emitting MEH-PPV into the TPU shell and coupling the turquoise blue-light-emitting perovskite NPs in the core site. Besides, large-scale fiber mats were fabricated using a commercially available electrospinning equipment with a rotary fiber collector. Finally, the orange-light-emitting nanofiber was incorporated into the polyfluorene (PFO)based emissive layer to form a white-light-emitting LED device. This work provided an effective way to prepare stable and stretchable luminous nanofibers and integration of such
2. RESULTS AND DISCUSSION We would like to develop stretchable perovskite nanofibers with the characteristics of uniformly luminous feature, mechanical endurance, and ambient stability. To this end, a thermoplastic polyurethane (TPU) was used as the fiber shell materials, comprising the urethane moiety in the main chain that connects to both hard and soft functional segments (Figure 1). In addition, it is nontoxic and biocompatible and
Figure 1. Schematical illustration of the coaxial electrospinning setup and the fabricated stretchable core−shell TPU/perovskite luminous nanofibers.
possesses a hydrophobic nature. More importantly, the constituent urethane group of TPU might form certain interactions with the Pb atom or methyl ammonium (CH3+) cation of perovskite materials to modulate the associated crystal growth.43 Regarding these features, we thus selected TPU as the polymer matrix for our electrospinning process. Prior to fabricating core−shell perovskite/polymer nanofibers, a typical uniaxial electrospinning process was first conducted to prepare the nanofibers and the obtained nanofibers were named as MAPbBr 3 -Uni (MA + = CH3NH3+). However, such uniaxial perovskite/polymer nanofibers exhibited a low PLQY of 2.1% at 533 nm (green-light emission), which was inferior to most values reported for MAPbBr3 NPs. This deficiency is likewise due to the nonuniform aggregated morphology of the perovskite NPs inside the electrospun fibers. Figure S1 (Supporting Information, SI) shows the scanning electron microscope (SEM) images of the fabricated uniaxial nanofibers, in which salient perovskite aggregates are clearly observed at the fiber surface. Such inhomogeneous formation of the perovskite NPs might be attributed to the rapid nucleation of perovskite crystals during the uniaxial electrospinning process.41 On the one hand, the nonuniform distribution of perovskite NPs would degrade the homogeneity of the emitting light; on the other hand, the rapid crystal growth could engender the formation of defective states, which results in an increased nonradiative decay of charges to yield low PLQY. Moreover, the direct contact of the perovskite aggregates with ambient air led to its degradation to cause emission instability.44 23606
DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
Research Article
ACS Applied Materials & Interfaces Table 1. Preparation Conditions, Parameters, and Characteristics of the Fabricated Nanofibers sample MAPbBr3-Unia MAPbBr3-1b MAPbBr3-2b MAPbBr3-3b MAPbBr3-4b MAPbBr3-5b MAPbCl3-1b MAPbI3-1b MAPb(ClxBr1−x)3b MAPb(BrxI1−x)3b
MAX/PbX2 shell (polymer) concentration (mg/mL) core flow rate (mL/h) 1.5:1 1.5:1 3:1 3:1 3:1 3:1 1.5:1 1.5:1 2:1 2:1
150 150 150 150 120 120 150 150 150 150
N/A 0.1 0.1 0.01 0.1 0.01 0.01 0.01 0.01 0.01
PL peak position (nm) PLQY (%) 533 534 534 525 536 532 405 753 465 600
2.1 8.3 16.3 23.3 13.2 16.8 10 000)] were purchased from Sigma-Aldrich. All chemicals were used as received without any further purification. 4.2. Precursor Solution Preparation. To prepare the precursor solutions of MAPbBr3, MAPbI3, and MAPb(BrxI1−x)3, PbX2 and MAX were dissolved in DMF. Nevertheless, due to the low solubility of Clbased precursor solutions, MACl was mixed with PbBr2 and PbCl2 in a mixed solvent of DMSO/DMF at a volume ratio of 1:1 to prepare the precursor solutions of MAPb(ClxBr1−x)3 and MAPbCl3. The perovskite precursor was prepared by mixing PbX2 and MAX at desired compositions. To prepare the precursor solution of polymer, 23612
DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
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ACS Applied Materials & Interfaces
4.6. Characterization. Morphological analysis of the perovskite NPs within the prepared nanofiber was characterized using transmission electron microscopy (TEM, FEI Tecnai G2 T20). The diameter and morphology of the prepared nanofibers were characterized using a scanning electron microscope (JEOL JSM6510) after the samples were sputtered with platinum. The optical absorption spectra of the prepared nanofibers were recorded using a Hitachi U-4100 UV−visible spectrophotometer, and their photoluminescence (PL) emission spectra were measured by a Horiba Fluorolog-3 spectrometer system. Fluorescence optical microscope images were collected by a confocal laser microscope (Leica LCS SP5). Fourier transform infrared (FTIR) spectra of fibers were recorded by a PerkinElmer Spectrum-Two Fourier transform infrared (FTIR) spectrometer using the transmission technique in the range from 500 to 4000 cm−1. Differential scanning calorimetry (DSC) analysis was carried out on TA Instruments DSC 25. The stress− strain diagram was obtained by a Shimadzu EZ-SX texture analyzer. W-LED and LED device performances including current−voltage, luminescence curve, external quantum efficiency, and electroluminescence spectra were recorded by a spectrophotometer (PR670) coupled with Keithley 2400. All of the device measurements were conducted in ambient air at room temperature.
TPU was dissolved in a mixed solvent of DMF/THF (v/v 2:1) with a concentration of 150 mg/mL. For the uniaxial electrospinning process, both prepared TPU and perovskite solutions were directly mixed to give a final mixing ratio of perovskite to TPU as 10%. Note that for preparing the white-light-emitting fibers, 4.5 mg of MEH-PPV was added into the TPU precursor solution. To fabricate LED devices, the PFO precursor was prepared in chlorobenzene to yield a final concentration of 14 mg/mL. 4.3. Preparation of Regular Electrospun Fiber. The coaxial (core−shell) electrospinning process was performed by separately feeding the core and shell solutions to fabricate the core−shell fibers, similar to that reported in our previous work.41 Detailed schematic illustration of the coaxial (core−shell) electrospinning setup is presented in Figure 1. As shown, two syringes connected to a coaxial spinneret with diameters of 0.90 mm (for the inner one) and 1.25 mm (for the outer one) were used to feed solutions by two syringe pumps (KD Scientific Model 100). The flow rate of the shell precursor was kept at 1 mL/h, whereas the rate of the core solution was controlled in the range of 0.01−0.1 mL/h. To prepare the core−shell electrospun fibers, for which the perovskite NPs were confined in the core site by the outer polymer shell, the tip of the core needle was connected to a high-voltage power supply (chargemaster CH30P SIMCO) and a voltage was set at 16.6 kV. The nonwoven nanofibers were collected vertically with a fixed working distance (between the tip of the needle and the collector) of 20 cm. The whole electrospinning process was operated at room temperature (25 °C) with a relative humidity (RH) of 50%. For the regular uniaxial electrospinning process, the TPU/ perovskite blending solution was supplied to a single needle with an inner diameter of 0.84 mm by one syringe pump (KD Scientific Model 100) at a flow rate of 1 mL/h and operated under a voltage of 16.6 kV. Similar to the coaxial electrospinning process, the nanofibers were collected vertically with a working distance of 20 cm and proceeded in an ambient condition (25 °C and an RH of 50%). 4.4. Preparation of Large-Scale Electrospun Fibers. The large-scale fiber mats were fabricated by using a commercial FALCO FES-COL nanofiber electrospinning setup that operated in the horizontal direction. The solution was fed into a needle with an inner diameter of 0.84 mm by one syringe pump at a flow rate of 1 mL/h and operated under a voltage of 27.4 kV where the distance from the tip to the rotary collector is 15 cm for the uniaxial large-scale fiber mats, named as uniaxial TPU/Pero. To fabricate large-scale core−shell fiber mat, named as coaxial TPU/Pero, two syringes connected to respective needles with diameters of 0.64 mm (for the inner one) and 1.27 mm (for the outer one) were used to feed solutions fabricated by the same commercial FALCO FES-COL nanofiber electrospinning setup. The flow rate of the shell precursor was kept at 1.2 mL/h, whereas the rate of the core solution was controlled at 0.3 mL/h. The electrospinning device was operated under a voltage of 23.1 kV where the distance from the tip to the rotary collector is 15 cm. The other experimental and ambient parameters that are not specified are the same as previous electrospinning methods. 4.5. Preparation of the LED Device. The PFO-based LED devices was fabricated on the ITO/glass substrate. ITO substrates were precleaned sequentially using deionized water, acetone, and isopropyl alcohol, followed by ozone treatment for 20 min. After cleaning the substrate, a PEDOT:PSS layer (45−50 nm) was spincoated onto the ITO glass at 3000 rpm for 60 s and annealed at 130 °C for 15 min. PFO solution (14 mg/mL) in chlorobenzene was spincoated at 1000 rpm for 60 s in a glovebox. Afterward, calcium (Ca) and aluminum (Al) were thermally deposited onto the PFO active layer with thicknesses of 15 and 100 nm, respectively. The active area of the fabricated LED device is 0.2 × 0.2 cm2. To fabricate W-LED, orange-light-emitting (MAPb(BrxI1−x)3) aligned nanofibers were collected on the PEDOT:PSS spin-coated ITO/glass substrates. Afterward, PFO solution was spin-coated in a glovebox atmosphere and the rest of the process was followed similar to that for PFO-based LED device.
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ASSOCIATED CONTENT
S Supporting Information *
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsami.9b05527.
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SEM images of polymer/perovskite electrospun nanofibers, prepared core−shell MAPbBr3-1, MAPbBr3-2, MAPbBr3-3, MAPbBr3-4, and MAPbBr3-5 nanofibers; FTIR spectra; fluorescence microscopic images of MAPbBr3-3 nanofibers; photoluminescence spectra of samples; durability test of MAPb(ClxBr1−x)3 nanofibers; PL intensity of MAPbBr3-3; and LED I−V curves (PDF)
AUTHOR INFORMATION
Corresponding Author
*E-mail:
[email protected]. ORCID
Chu-Chen Chueh: 0000-0003-1203-4227 Wen-Chang Chen: 0000-0003-3170-7220 Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS The authors appreciate the financial supports by “Advanced Research Center for Green Materials Science and Technology” from the Featured Area Research Center Program within the framework of the Higher Education Sprout Project by the Ministry of Education (108L9006) and the Ministry of Science and Technology in Taiwan (MOST 107-3017-F-002-001 and MOST 108-2636-E-194-001).
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DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
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DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
Research Article
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DOI: 10.1021/acsami.9b05527 ACS Appl. Mater. Interfaces 2019, 11, 23605−23615
