Preparation and formation process of high efficient and stable CsPbBr3-Cs4PbBr6 nanocrystals with mixed phase

Chen Xue-Lian; Jiao Hu-Po; Shen Yan-Bing; Pan Xi-Qiang

doi:10.7498/aps.72.20230066

Abstract

CsPbBr₃-Cs₄PbBr₆ dual-phase nanocrystals are prepared by adding the mixture ligand of oleylamine and tetradecyl-phosphonic acid (OLA-TDPA) to CsPbBr₃ perovskite nanocrystals through ligand post-treatment. The structure, the morphology, optical property and the stability of CsPbBr₃-Cs₄PbBr₆ dual-phase nanocrystals are characterized by X-ray diffraction, transmission electron microscopy (high-resolution TEM), UV-vis spectrophotometer, fluorescence spectrophotometer, and transient fluorescence spectrophotometer. The as-obtained nanocrystals have a high photoluminescence quantum yield of 78% and long fluorescence lifetime of 476 ns when prepared at the optimal molar ratio of CsPbBr₃, TDPA and OLA (1∶1∶15). Moreover, the nanocrystal is quite stable at room temperature for at least 25 days, and has a good thermal stability in five heating-cooling cycles at temperature in a range between 293 K and 328 K. The formation of dual-phase nanocrystals go through two stages of surface passivation/dissolution and recrystallization to generate CsPbBr₃-Cs₄PbBr₆ nanocrystals. In the first stage (t ≤ 1 h), the m OLA-TDPA mixing ligand can form (RNH₃)₂PO₃ X type ligand and exchanges with [RNH₃]⁺-[RCOO]^– at the surface of CsPbBr₃ nanocrystals, which can effectively passivate surface defects by strong interaction with Pb²⁺ and high ligand content at surface, thus improving the quantum yield and fluorescence life of CsPbBr₃ nanocrystals with spherical shape. In the second stage, with the increase of reaction time, PbBr₂ partially dissolves from the surface of CsPbBr₃ nanocrystals, then some CsPbBr₃ nanocrystals transform into lead-depleted Cs₄PbBr₆ nanocrystals with hexagonal phase, thus improving the stability of nanocrystals. This work has a certain reference value for promoting the applications of high efficient and stable perovskite nanocrystals.

Keywords:

Authors and contacts

1.
School of Materials Science and Engineering, Xi’an Shiyou University, Xi’an 710065, China
2.
College of Chemistry and Chemical Engineering, Xi’an Shiyou University, Xi’an 710065, China

Corresponding author: Chen Xue-Lian, chenxl@xsyu.edu.cn ; Pan Xi-Qiang, pxq2336@163.com

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 62104191) and the Postgraduate Innovation and Practical Ability Training Program of Xi’an Shiyou University, China (Grant No. YCS21112073).

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Cited By

图 1 CsPbBr₃ NCs和OLA-TDPA-PNCs的 X 射线衍射图

Figure 1. X-ray diffraction patterns of CsPbBr₃ NCs and OLA-TDPA-PNCs.

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图 2 CsPbBr₃ NCs的TEM图像(a)及其对应的HRTEM图(b); OLA-TDPA-PNCs 的TEM图像(c)及其对应的HRTEM图(d)和(e)

Figure 2. TEM image of CsPbBr₃ NCs (a) and the corresponding HRTEM image (b); TEM image of OLA-TDPA-PNCs (c) and the corresponding HRTEM images (d) and (e).

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图 3 (a) CsPbBr₃ NCs和OLA-TDPA-PNCs在日光照射(上)和365 nm紫外照射下(下)的实物照片; CsPbBr₃ NCs和OLA-TDPA-PNCs 的PL图谱(b)、UV-vis图谱(c)和时间衰减曲线(d)

Figure 3. (a) Photographs of CsPbBr₃ NCs and OLA-TDPA-PNCs under ambient light (top) and 365 nm UV irradiation (bottom); PL spectra (b), UV-vis absorption spectra (c), and time-resolved PL decay curves (d) of pristine CsPbBr₃ NCs and OLA-TDPA-PNCs in hexane.

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图 4 (a)在紫外灯的连续照射下, CsPbBr₃ NCs和OLA-TDPA-PNCs的相对PL强度随光照时间的变化; (b)在常温密封条件下连续监测CsPbBr₃ NCs和OLA-TDPA-PNCs的相对PL强度, 持续时间长达26 d; (c) CsPbBr₃ NCs和OLA-TDPA-PNCs在298—328 K时的相对PL强度变化; (d) OLA-TDPA-PNCs在经历5次加热-冷却循环的相对PL强度变化

Figure 4. Variations of relative PL intensity of pristine CsPbBr₃ NCs and OLA-TDPA-PNCs under continuous UV 365 nm illumination (a); and stored under ambient conditions with sealing (b). Change of relative PL intensity of CsPbBr₃ NCs and OLA-TDPA-PNCs between 298 and 328 K (c); change of relative PL intensity of OLA-TDPA-PNCs recorded during 5 heating-cooling cycles between 298 and 328 K (d).

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图 5 OLA, TDPA, OLA-TDPA , OLA-TDPA-PNCs, TDPA-PNCs和CsPbBr₃ NCs的FTIR光谱　(a) 800—1800 cm^–1; (b) 2000—3500 cm^–1

Figure 5. FTIR spectra of OLA, TDPA, OLA-TDPA , OLA-TDPA-PNCs, TDPA-PNCs and CsPbBr₃ NCs at 800–1800 cm^–1 (a) and (b) 2000–3500 cm^–1

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图 6 OLA-TDPA-PNCs (上), TDPA-PNCs (中)和CsPbBr₃ NCs (下)的XPS光谱图全谱(a), 以及Cs 3d (b), Pb 4f (c), Br 3d (d), N 1s (e), P 2p (f)的XPS核级谱

Figure 6. Survey XPS spectra (a), XPS core level spectra of Cs 3d (b), Pb 4f (c), Br 3d (d), N 1s (e) and P 2p (f) of OLA-TDPA-PNCs (top), TDPA-PNCs (middle) and CsPbBr₃ NCs (bottom).

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图 7 OLA-TDPA- PNCs随时间变化的光学监测　(a) UV-vis吸收光谱; (b)荧光光谱, 内插图为纳米晶在1—96 h间的荧光光谱图

Figure 7. Optical monitoring of the OLA-TDPA- PNCs over time: (a) UV-vis absorption spectra; (b) PL spectra, inset shows the PL spectra of OLA-TDPA- PNCs between 1 and 96 h.

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表 1 CsPbBr₃ NCs和OLA-TDPA-PNCs的荧光寿命拟合

Table 1. Lifetime and fractional contribution of different decay channels for samples of CsPbBr₃ NCs and OLA-TDPA-PNCs.

Sample τ₁/ns τ₂/ns τ₃/ns K_nr/(10⁶ s^–1) K_r/(10⁶ s^–1) K_nr/K_r τ_avg/ns PLQY/%

CsPbBr₃ NCs 6.83 42.13 277.42 5.48 0.97 5.65 155 15
OLA-TDPA-PNCs 12.56 79.07 824.81 0.47 1.64 0.29 476 78

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[1]	Uddin M A, Mobley J K, Masud A A, Liu T, Calabro R L, Kim D Y, Richards C I, Graham K R 2019 J. Phys. Chem. C 123 18103 Google Scholar
[2]	Nedelcu G, Protesescu L, Yakunin S, Bodnarchuk M I, Grotevent M J, Kovalenko M V 2015 Nano Lett. 15 5635 Google Scholar
[3]	陈雪莲, 巨博, 焦琥珀, 李燕, 钟玉洁 2022 物理学报 71 096802 Google Scholar Chen X L, Ju B, Jiao H P, Li Y, Zhong Y J 2022 Acta Phys. Sin. 71 096802 Google Scholar
[4]	Meyns M, Peralvarez M, Heuer-Jungemann A, Hertog W, Ibanez M, Nafria R, Genc A, Arbiol J, Kovalenko M V, Carreras J, Cabot A, Kanaras A G 2016 ACS Appl. Mater. Interfaces 8 19579 Google Scholar
[5]	Liu P Z, Chen W, Wang W G, Xu B, Wu D, Hao J J, Cao W Y, Fang F, Li Y, Zeng Y Y, Pan R K, Chen S M, Cao W Q, Sun X W, Wang K 2017 Chem. Mater. 29 5168 Google Scholar
[6]	Li S, Shi Z F, Zhang F, Wang L T, Ma Z Z, Yang D W, Yao Z Q, Wu D, Xu T T, Tian Y T, Zhang Y T, Shan C X, Li X J 2019 Chem. Mater. 31 3917 Google Scholar
[7]	Wang Y R, Zhang M, Xiao K, Lin R X, Luo X, Han Q L, Tan H R 2020 J. Semicond. 41 051201 Google Scholar
[8]	林月明, 巨博, 李燕, 陈雪莲 2021 物理学报 70 128803 Google Scholar Lin M Y, Ju B, Li Y, Chen X L 2021 Acta Phys. Sin. 70 128803 Google Scholar
[9]	Li J Z, Dong H X, Xu B, Zhang S F, Cai Z P, Wang J, Zhang L 2017 Photonics Res. 5 457 Google Scholar
[10]	Sun S B, Yuan D, Xu Y, Wang A F, Deng Z T 2016 ACS Nano 10 3648 Google Scholar
[11]	De Roo J, De Keukeleere K, Hens Z, Van Driessche I 2016 Dalton Trans. 45 13277 Google Scholar
[12]	Xiao M, Hao M, Lyu M, Moore E G, Zhang C, Luo B, Hou J, Lipton-Duffin J, Wang L 2019 Adv. Funct. Mater. 29 1905683 Google Scholar
[13]	Han D B, Imran M, Zhang M J, Chang S, Wu X G, Zhang X, Tang J L, Wang M S, Ali S, Li X G, Yu G, Han J B, Wang L X, Zou B S, Zhong H Z 2018 ACS Nano 12 8808 Google Scholar
[14]	Krieg F, Ochsenbein S T, Yakunin S, Ten Brinck S, Aellen P, Suess A, Clerc B, Guggisberg D, Nazarenko O, Shynkarenko Y, Kumar S, Shih C J, Infante I, Kovalenko M V 2018 ACS Energy Lett. 3 641 Google Scholar
[15]	Pan J, Shang Y, Yin J, De Bastiani M, Peng W, Dursun I, Sinatra L, El-Zohry A M, Hedhili M N, Emwas A H, Mohammed O F, Ning Z, Bakr O M 2018 J. Am. Chem. Soc. 140 562 Google Scholar
[16]	Bi C H, Kershaw S V, Rogach A L, Tian J J 2019 Adv. Funct. Mater. 29 1902446 Google Scholar
[17]	Park S, Cho H, Choi W, Zou H, Jeon D Y 2019 Nanoscale Adv. 1 2828 Google Scholar
[18]	Li Z J, Hofman E, Li J, Davis A H, Tung C H, Wu L Z, Zheng W 2017 Adv. Funct. Mater. 28 1704288 Google Scholar
[19]	Qiao B, Song P J, Cao J, Zhao S L, Shen Z, Di G, Liang Z Q, Xu Z, Song D, Xu X R 2017 Nano Energy 28 445602 Google Scholar
[20]	Quan L N, Quintero-Bermudez R, Voznyy O, Walters G, Jain A, Fan J Z, Zheng X, Yang Z, Sargent E H 2017 Adv. Mater. 29 1605945 Google Scholar
[21]	Palazon F, Dogan S, Marras S, Locardi F, Nelli I, Rastogi P, Ferretti M, Prato M, Krahne R, Manna L 2017 J. Phys. Chem. C 121 11956 Google Scholar
[22]	Liang W C, Li T, Zhu C C, Guo L D 2022 Optik 267 169705 Google Scholar
[23]	Peng X G, Chen J, Wang F C, Zhang C Y, Yang B B 2020 Optik 208 164579 Google Scholar
[24]	Su Y, Zeng Q H, Chen X J, Ye W G, She L S, Gao X M, Ren Z Y, Li X M 2019 J. Mater. Chem. C 7 7548 Google Scholar
[25]	Akkerman Q A, Abdelhady A L, Manna L 2018 J. Phys. Chem. Lett. 9 2326 Google Scholar
[26]	Nie Z H, Gao X Z, Ren Y J, Xia S Y, Wang Y H, Shi Y L, Zhao J, Wang Y 2020 Nano Lett. 20 4610 Google Scholar
[27]	Natalia R, Mingrui Y, Paul G, Natalia K, Pavel M, Eckard H, Luis R R, Dmitry P, Dmitriy K, Zamkov M 2018 Chem. Mater. 30 1391 Google Scholar
[28]	Akkerman Q A, Park S, Radicchi E, Nunzi F, Mosconi E, De Angelis F, Brescia R, Rastogi P, Prato M, Manna L 2017 Nano Lett. 17 1924 Google Scholar
[29]	Li F, Liu Y, Wang H L, Zhan Q, Liu Q L, Xia Z G 2018 Chem. Mater. 30 8546 Google Scholar
[30]	Wang L, Liu H, Zhang Y, Mohammed O F 2020 ACS Energy Lett. 5 87 Google Scholar
[31]	Liang Z Q, Zhao S L, Xu Z, Qiao B, Song P J, Gao D, Xu X R 2016 ACS Appl. Mater. Interfaces 8 28824 Google Scholar
[32]	Vallés-Pelarda M, Gualdrón-Reyes A F, Felip-León C, Angulo-Pachón C A, Agouram S, Muñoz-Sanjosé V, Miravet J F, Galindo F, Mora-Seró I 2021 Adv. Opt. Mater. 9 2001786 Google Scholar
[33]	Xuan T T, Yang X F, Lou S Q, Huang J J, Liu Y, Yu J B, Li H L, Wong K L, Wang C X, Wang J 2017 Nanoscale 9 15286 Google Scholar
[34]	Zhang C, Lian L Y, Zhang J B, Su X M, Liu S S, Gao Y L, Lian Z Y, Sun D Z, Luo W, Zheng H M, Zhang D L 2022 J. Phys. Chem. C 126 4172 Google Scholar
[35]	De Roo J, Ibanez M, Geiregat P, Nedelcu G, Walravens W, Maes J, Martins J C, Van Driessche I, Kovalenko M V, Hens Z 2016 ACS Nano 10 2071 Google Scholar
[36]	Luschtinetz R, Seifert G, Jaehne E, Adler H J P 2007 Macromol. Symp. 254 248 Google Scholar
[37]	Son J G, Choi E, Piao Y, Han S W, Lee T G J N 2016 Nanoscale 8 4573 Google Scholar
[38]	Sun W, Yun R, Liu Y, Zhang X, Yuan M, Zhang L, Li X 2023 Small 19 2205950 Google Scholar
[39]	Wei Y, Cheng Z, Lin J 2019 Chem. Soc. Rev. 48 310 Google Scholar
[40]	Liu Z, Bekenstein Y, Orcid X Y, Nguyen S C, Orcid J S, Orcid D Z, Lee S T, Orcid P Y, Orcid W M, Alivisatos A P 2017 J. Am. Chem. Soc. 139 5309 Google Scholar

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Preparation and formation process of high efficient and stable CsPbBr₃-Cs₄PbBr₆ nanocrystals with mixed phase

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Corresponding author: Chen Xue-Lian, chenxl@xsyu.edu.cn ; Pan Xi-Qiang, pxq2336@163.com

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Sample	τ₁/ns	τ₂/ns	τ₃/ns	K_nr/(10⁶ s^–1)	K_r/(10⁶ s^–1)	K_nr/K_r	τ_avg/ns	PLQY/%
CsPbBr₃ NCs	6.83	42.13	277.42	5.48	0.97	5.65	155	15
OLA-TDPA-PNCs	12.56	79.07	824.81	0.47	1.64	0.29	476	78

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