Ni<sup>2+</sup>掺杂和卤素空位填充协同抑制CsPbBr<sub>3</sub>纳米晶体中的离子迁移 -

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Ni²⁺掺杂和卤素空位填充协同抑制CsPbBr₃纳米晶体中的离子迁移

doi:10.37188/CO.2020-0060

孙智国^{1, 2,},
吴晔^{1, 2},
魏昌庭^{1, 2},
耿冬苓^{1, 2},
李晓明^{1, 2,,},
曾海波^{1, 2,,}

1.
南京理工大学材料科学与工程学院，江苏南京 210094
2.
南京理工大学新型显示材料与器件工信部重点实验室纳米光电材料研究所，江苏南京 210094

基金项目:中国科协青年精英科学家资助项目(No. 2018QNRC001)；国家自然科学基金(No. 61874054、No. 51902160)；江苏省自然科学基金(No. BK20180489)、中央高校基础研究基金(No. 30918011208)；国家杰出青年自然科学基金(No. 61725402)

详细信息

作者简介:
孙智国（1988—），男，贵州毕节人，南京理工大学博士研究生在读，主要从事光电材料的合成及性能的研究。E-mail：sunzhiguo@njust.edu.cn
李晓明 (1991—)，男，江苏扬州人，南京理工大学教授，2017年于南京航空航天大学获得材料科学博士学位，主要从事卤化物钙钛矿合成及光电应用的研究。E-mail:lixiaoming@njust.edu.cn
曾海波（1977—），男，湖北鄂州人，博士，教授，南京理工大学材料学院院长，杰青，主要从事半导体的光电应用的研究。E-mail：zeng.haibo@njust.edu.cn

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出版历程
- 收稿日期:2020-04-13
- 修回日期:2020-05-11
- 网络出版日期:2020-12-25
- 刊出日期:2021-01-25

Suppressed ion migration in halide perovskite nanocrystals by simultaneous Ni²⁺doping and halogen vacancy filling

SUN Zhi-guo^{1, 2,},
WU Ye^{1, 2},
WEI Chang-ting^{1, 2},
GENG Dong-ling^{1, 2},
LI Xiao-ming^{1, 2,,},
ZENG Hai-bo^{1, 2,,}

1.
School of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094, China
2.
Institute of Optoelectronics and Nanomaterials, MIIT Key Laboratory of Advanced Display Materials and Devices, Nanjing University of Science and Technology, Nanjing 210094, China

Funds:Supported by Young Elite Scientists Sponsorship Program by CAST (No. 2018QNRC001), National Natural Science Foundation of China (No. 61874054, No. 51902160), Natural Science Foundation of Jiangsu Province (No. BK20180489), Fundamental Research Funds for the Central Universities (No. 30918011208), National Natural Science Funds for Distinguished Young Scholar (No. 61725402)

More Information

Corresponding author:lixiaoming@njust.edu.cn;zeng.haibo@njust.edu.cn

摘要

摘要:卤化铅钙钛矿(LHPs)由于具有优异的光电性能和制备成本低等优点，已成为新一代光电器件的有力候选材料。然而，缺陷造成的离子迁移会导致LHPs纳米晶的晶体结构解离分解。因此，稳定性成为LHPs实际应用中亟待解决的问题。本文旨在研究镍离子替位掺杂及卤素空位填补对CsPbBr ₃纳米晶中的离子迁移抑制作用。通过离子迁移活化能的测定和高分辨透射电镜的原位观察，分析了前驱体掺杂剂对加强LHPs稳定性的作用原理。首先，选用乙酰丙酮镍和溴化镍作为掺杂剂，合成了掺杂LHPs纳米晶。其次，通过吸收-荧光光谱，X射线衍射，X射线光电子衍射，透射电子显微镜等测试手段对掺杂样品的光学及化学组成进行分析。最后，通过纳米晶薄膜电导率的温度依赖关系计算出其离子迁移活化能，并结合高分辨电镜原位观察纳米晶在高能电子束辐照下的形貌演变过程，揭示了不同掺杂剂对合成掺杂LHPs稳定性的影响。实验结果表明：Ni ²⁺掺杂CsPbBr ₃样品的离子迁移活化能相较本征CsPbBr ₃样品（0.07 eV）有显著提升，其中乙酰丙酮镍掺杂样品的离子迁移活化能为0.238 eV，溴化镍掺杂样品的离子迁移活化能为0.487 eV。另外，电子束辐照测试表明溴化镍掺杂钙钛矿晶体表现出更高的结构稳定性，这主要归因于掺杂的Ni ²⁺对卤素的强结合和卤素填补空位缺陷的协同钝化作用。Ni ²⁺掺杂和卤素空位填充协同可以有效抑制卤化物钙钛矿纳米晶体中的离子迁移。
- 铅卤钙钛矿/
- 掺杂/
- 离子迁移活化能/
- 电子束辐照/
- 稳定性
Abstract:Lead Halide Perovskites(LHPs) are promising candidates for next-generation optoelectronic application. However, defect-induced ion migration causes phase degradation in LHP nanocrystals. Therefore, material stability has become an urgent problem that impedes practical applications. In this paper, we aim to study the influence of doping cations on inhibiting the migration of halogen ions in perovskite nanocrystals. Through the measurement of ion migration activation energy and in-situ high-resolution transmission electron microscope technology, the effect of precursor dopants on the stability of LHPs were analyzed. Firstly, we synthesized two types of LHP nanocrystals with high crystal quality using nickel acetylacetonate and nickel bromide as precursor dopants, respectively. Secondly, the optical properties and component elements of the doped samples were analyzed by absorption-fluorescence spectroscopy, X-ray diffraction, X-ray photoelectron diffraction, and transmission electron microscopy. Finally, the ion migration activation energies of various LHP films were measured using temperature-dependent ion conductivity tests, and the influence of the precursor dopants on the stability of as-synthesized doped LHPs was compared with the results from high-resolution electron microscopy. The results showed that the activation energies of the doped CsPbBr ₃samples were significantly improved compared to the intrinsic CsPbBr ₃sample (0.07 eV), which were determined to be 0.238 eV for nickel acetylacetonate and 0.487 eV for nickel bromide. In addition, the electron irradiation experiments showed that the nickel bromide-doped perovskite nanocrystals exhibited higher structural stability. This is due to the strong bonding of doped Ni ²⁺to halogen and the synergistic passivation effect of halogen filling vacancy defects. It can be concluded that Ni ²⁺doping and halogen vacancy filling can effectively inhibit ion migration in halide perovskite nanocrystals.
- lead halide perovskite/
- doping/
- ion migration activation energy/
- electron beam irradiation/
- stability

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图 1钙钛矿样品的结构和性能。（a, b）为溴化镍掺杂（NiBr₂-doped）CsPbBr₃纳米晶的吸收光谱和发射光谱。(c, d) 乙酰丙酮镍掺杂（Ni(acac)₂-doped））CsPbBr₃纳米晶吸收光谱和发射光谱。（e, f, g）分别为未掺杂，乙酰丙酮镍掺杂及溴化镍掺杂CsPbBr₃纳米晶体TEM图像。(h) 掺Ni的CsPbBr₃纳米晶与本征CsPbBr₃的XPS图谱。 (i,k)分别为NiBr₂-doped、Ni(acac)₂-doped CsPbBr₃纳米晶的XRD图谱，在图的底部显示了斜方CsPbBr₃结构。（j, l）分别为Ni(acac)₂-doped、NiBr₂-doped CsPbBr₃纳米晶的高分辨XRD谱(110)（JCPDS No.18-0364）

Figure 1.Structures and properties of LHPs. Absorption spectra and PL spectra of CsPbBr₃nanocrystals doped with NiBr₂(a, b) and Ni(acac)₂(c,d). (e, f, g) TEM images of Ni-doped and undoped CsPbBr₃nanocrystals. (h) XPS spectra of Ni-doped and undoped CsPbBr₃nanocrystals. (i, k) XRD patterns of NiBr₂-doped, Ni(acac)₂-doped and undoped CsPbBr₃nanocrystals. JCPDS No.18-0364 of the orthorhombic CsPbBr₃structure are indicated at the bottom of each figure. (j, l) High-resolution XRD spectra (110) of NiBr₂-doped, Ni(acac)₂-doped and undoped CsPbBr₃nanocrystals

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图 2电子束辐照实验结果及原理图

Figure 2.Experimental results of electron beam irradiation and corresponding schematic diagram

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图 3活化能测试示意图及测试结果。（a）活化能测试示意图，图中t₁和t₂指光电流和暗电流分别拟合得到的光/暗电流的驰豫时间。（b）不同温度暗电流变化（NiBr₂掺杂10%），插图显示以电流弛豫时间为横坐标的半对数暗电流曲线（lnA）。（c）阿伦尼乌斯关系式活化能(E_a)计算结果。（d）不同掺杂样品的活化能 (x代表实际含量)

Figure 3.Schematic diagram of activation energy test and test results. (a) Schematic diagram of activation energy test.t₁andt₂in the figure refer to the relaxation time of the light/dark currents fitted by the photocurrent and dark current, respectively. (b) The dark current changes at different temperatures (NiBr₂doping 10%). The inset shows the semilog dark current (lnA) curve as function with the current relaxation time. (c) Activation energy (E_a) caculated by formla (1). (d) Activation energy of different doped samples (xis the actual content)

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图 4掺杂与空位填补原理图。（a）掺杂锚定；（b）空位填补

Figure 4.Schematic diagram of doping and vacancy filling. (a) Doping anchoring; (b) vacancy filling

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表 1使用ICP-MS测试的掺杂含量

Table 1.Doping content tested by ICP-MS

乙酰丙酮镍掺杂		溴化镍掺杂
名义含量	实际含量*	名义含量	实际含量
5%	0.07	5%	0.11
10%	0.12	10%	0.14
12%	0.13	12%	0.17
15%	0.20	15%	0.21
20%	0.23	20%	0.25
*：表示ICP-MS测定的CsPb_1−xNi_xBr₃中Ni掺杂的实际含量

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