具有可调谐和长寿命荧光发射的高亮度、单分散四元CuInZnS@ZnS量子点

doi:10.15541/jim20240426

无机材料学报 ›› 2025, Vol. 40 ›› Issue (4): 433-339.DOI: 10.15541/jim20240426 CSTR: 32189.14.10.15541/jim20240426

具有可调谐和长寿命荧光发射的高亮度、单分散四元CuInZnS@ZnS量子点

陈梓¹(), 张爱迪¹^,²(), 龚克², 刘海华¹, 禹钢³, 单青松⁴, 刘勇², 曾海波⁴()

1.淮阴工学院化学工程学院, 江苏省凹土资源利用重点实验室, 淮安 223003
2.南京贝迪新材料科技股份有限公司, 南京 211103
3.北京大学北京分子科学国家研究中心, 化学与分子工程学院, 北京 100871
4.南京理工大学材料科学与工程学院, 新型显示材料与器件工信部重点实验室, 南京 210094

收稿日期:2024-10-08 修回日期:2024-11-15 出版日期:2025-04-20 网络出版日期:2024-12-16
通讯作者: 张爱迪, 高级工程师. E-mail: zhangaidi@bready.cn;
曾海波, 教授. E-mail: zeng.haibo@njust.edu.cn
作者简介:陈梓(1985-), 女, 博士. E-mail: chenzi@hyit.edu.cn

High-brightness and Monodisperse Quaternary CuInZnS@ZnS Quantum Dots with Tunable and Long-lived Emission

CHEN Zi¹(), ZHANG Aidi¹^,²(), GONG Ke², LIU Haihua¹, YU Gang³, SHAN Qingsong⁴, LIU Yong², ZENG Haibo⁴()

1. Key Laboratory for Palygorskite Science and Applied Technology of Jiangsu Province, Faculty of Chemical Engineering, Huaiyin Institute of Technology, Huaian 223003, China
2. Nanjing Bready Advanced Materials Technology Co., Ltd., Nanjing 211103, China
3. Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China
4. MIIT Key Laboratory of Advanced Display Materials and Devices, School of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094, China

Received:2024-10-08 Revised:2024-11-15 Published:2025-04-20 Online:2024-12-16
Contact: ZHANG Aidi, senior engineer. E-mail: zhangaidi@bready.cn;
ZENG Haibo, professor. E-mail: zeng.haibo@njust.edu.cn
About author:CHEN Zi (1985-), female, PhD. E-mail: chenzi@hyit.edu.cn
Supported by:
Fund Project for Transformation of Scientific and Technological Achievements of Jiangsu Province of China(BA2023020)

摘要/Abstract

摘要：

作为环境友好型发光量子点(QDs)的重要替代材料, CuInS基核/壳量子点近年来受到越来越多的关注。然而, 这类量子点的一些缺点仍然阻碍了它们的工业化应用, 比如较低的光致发光量子产率(PLQY)、复杂的合成途径、发射光谱易失去控制、光稳定性不足等。本研究通过一锅/三步法合成策略成功制备了CuInZnS@ZnS核/壳量子点, 并精确调控其荧光发射光谱, 然后系统研究了CuInZnS@ZnS量子点在晶核形成、合金化和ZnS壳层生长过程中的集合体光谱特性。通过控制Cu/In元素的化学计量比、Zn²⁺掺杂以及ZnS壳层生长, 实现了量子点荧光发射峰在530~850 nm范围内的精准调控。CuInZnS@ZnS量子点具有明显的长荧光发射寿命(长达750 ns)、高PLQY(高达85%)和优异的结晶度。基于Cu缺陷相关的分子内定域能级发射模型阐释了集合体光谱演变规律。通过控制Cu/In元素的化学计量比, 并且基于Cu缺陷的不同氧化态, 提出了两种不同的Cu缺陷相关发射途径。本工作为制备高荧光效率的三元或四元合金量子点提供了更深入的见解。

关键词: 量子点, 铜铟硫, 合金, 核壳, 集合体光谱, Cu缺陷发光

Abstract:

As an essential candidate for environment-friendly luminescent quantum dots (QDs), CuInS-based QDs have attracted more attention in recent years. However, several drawbacks still hamper their industrial applications, such as lower photoluminescence quantum yield (PLQY), complex synthetic pathways, uncontrollable emission spectra, and insufficient photostability. In this study, CuInZnS@ZnS core/shell QDs was prepared via a one-pot/three-step synthetic scheme with accurate and tunable control of PL spectra. Then their ensemble spectroscopic properties during nucleation formation, alloying, and ZnS shell growth processes were systematically investigated. PL peaks of these QDs can be precisely manipulated from 530 to 850 nm by controlling the stoichiometric ratio of Cu/In, Zn²⁺ doping and ZnS shell growth. In particular, CuInZnS@ZnS QDs possess a significantly long emission lifetime (up to 750 ns), high PLQY (up to 85%), and excellent crystallinity. Their spectroscopic evolution is well validated by Cu-deficient related intragap emission model. By controlling the stoichiometric ratio of Cu/In, two distinct Cu-deficient related emission pathways are established based on the differing oxidation states of Cu defects. Therefore, this work provides deeper insights for fabricating high luminescent ternary or quaternary-alloyed QDs.

Key words: quantum dot, CuInS, alloying, core/shell, ensemble spectroscopic, Cu-deficient related emission

中图分类号:

TQ174

陈梓, 张爱迪, 龚克, 刘海华, 禹钢, 单青松, 刘勇, 曾海波. 具有可调谐和长寿命荧光发射的高亮度、单分散四元CuInZnS@ZnS量子点[J]. 无机材料学报, 2025, 40(4): 433-339.

CHEN Zi, ZHANG Aidi, GONG Ke, LIU Haihua, YU Gang, SHAN Qingsong, LIU Yong, ZENG Haibo. High-brightness and Monodisperse Quaternary CuInZnS@ZnS Quantum Dots with Tunable and Long-lived Emission[J]. Journal of Inorganic Materials, 2025, 40(4): 433-339.

图/表 21

Fig. 1 Optical and morphology characterization of the CuInS-based QDs (a) Synthetic route of the CuInS-based QDs; (b) Photograph of the CuInZnS@ZnS QDs with shell growth of 20 h (Cu : In : Zn is 1 : 2 : 3) under 365 nm showing brilliant luminescence; (c) Transient PL decays of the CuInZnS@ZnS QDs with different shell growth time (Cu : In : Zn is 1 : 2 : 3); (d) TEM images of the CuInZnS/ZnS QDs (Cu : In : Zn is 1 : 2 : 3) with shell growth of 20 h. Colorful figures are available on website

Fig. 2 Schematic depictions of relaxation processes in stoichiometric CuInS QDs (a), Cu-deficient CuInS QDs (b), and Cu-deficient CuInZnS@ZnS core/shell QDs (c) (a) Photon absorption is mainly due to the VB to CB transition. For the CuInS QDs with Cu/In ratio close to stoichiometric, the PL emission was due to radiative recombination of the CB electron with the hole existing in the intragap Cu+ state. (b) For the Cu-deficient CuInS QDs, there are three main processes. Process ①: a hole existing in the ground state forms Cu2+ defect, and it can directly recombine with the CB electron. Process ②: the recombination process was slow with the lifetime lasting hundreds of nanoseconds. To dominate the PL emission, another Cu vacancy trap (noted as VCu) quickly captured the photogenerated hole from the VB state, and formed a charge-compensated pair with the Cu2+ defect. Process ③: the trapped hole at VCu center radiatively recombined with the electron and finished the whole recombination process. (c) For the Cu-deficient core/shell QDs, the diffusion of Zn2+ ions occupied and decreased the VCu intragap states, and the thick ZnS shell eliminated the electron trap bands associated with the CB. The recombination of hot electron at CB edge and hole located at the intragap state (Cu+) dominated the PL decay process.

Fig. S1 Synthetic equipment of the CuInS-based QDs

Fig. S2 Digital photographs of CuInS QDs in a typical nucleation growth process under daylight lamp and UV lamp (365 nm) DDT was chosen as the sulfur source, surface ligand, and solvent. The reaction temperature was 200 ℃

Fig. S3 Digital photographs of CuInS QDs in a typical nucleation growth process under daylight lamp and UV lamp (320 nm)

Fig. S4 Temporal evolution of PL emission spectra of CuInS QDs synthesized with different molar stoichiometric ratios of Cu : In precursors (a-d) stand for 1 : 1, 1 : 2, 1 : 4, and 1 : 6. DDT was chosen as the sulfur source. The aliquots of QDs samples for the PL intensity test were fixed. PL spectra were recorded with excitation at 450 nm

Fig. S5 Temporal evolution of PL spectra of CuInS QDs, CuInZnS QDs, and CuInZnS@ZnS QDs with different growth time (a-d) stand for the stoichiometric ratio of Cu : In at 1 : 1, 1 : 2, 1 : 4, and 1 : 6. PL spectra were recorded with excitation at 450 nm

Fig. S6 Temporal evolution of UV-Vis absorption spectra of CuInS QDs, CuInZnS QDs, CuInZnS@ZnS QDs synthesized with different molar stoichiometric ratios of Cu : In precursors (a-d) stand for the stoichiometric ratio of Cu : In at 1 : 1, 1 : 2, 1 : 4, and 1 : 6. The absorption shoulder/onset is more blue-shifted with less Cu/In ratio

Fig. S7 Temporal evolution of PL central emission peaks for CuInZnS@ZnS QDs with different shell growth time The stoichiometric ratios of Cu : In are 1 : 1, 1 : 2, 1 : 4, and 1 : 6

Fig. S8 Temporal evolution of PLQY for CuInZnS@ZnS QDs with different shell growth time The stoichiometric ratios of Cu : In are 1 : 1, 1 : 2, 1 : 4, and 1 : 6

Fig. S9 Representative transient PL decays for CuInZnS QDs The stoichiometric ratios of Cu : In are 1 : 1, 1 : 2, 1 : 4, and 1 : 6

Fig. S10 Representative transient PL decays of CuInZnS@ZnS QDs with different ZnS shell growth time The stoichiometric ratio of Cu : In is 1 : 4

Fig. S11 TEM image of CuInS QDs (the stoichiometric ratio of Cu : In at 1 : 2) with reaction time of 30 min The red triangle frames indicate the shapes of the CuInS QDs

Fig. S12 TEM image of CuInZnS QDs (the stoichiometric ratio of Cu : In : Zn at 1 : 2 : 3) with Zn etching time of 90 min The red triangle frames indicate the shapes of the CuInZnS QDs

Fig. S13 TEM images of CuInZnS@ZnS QDs (the stoichioetric ratio of Cu : In : Zn at 1 : 2 : 3) with ZnS shell growth time of 5 h The insert showing their representative high- esolution TEM images

Fig. S14 Size distribution histograms for CuInZnS/ZnS QDs (Cu : In : Zn at 1 : 2 : 3) with shell growth of 20 h To build the histograms, over 100 particles were measured

Fig. S15 XRD patterns of CuInS QDs (Cu : In stoichiometric ratio at 1 : 2) and (Zn)CuInS/ZnS QDs (Cu : In : Zn stoichioetric ratio at 1 : 2 : 3)

Table S1 Relevant parameters for CuInS QDs synthesized with different molar stoichiometric ratios of Cu : In. λem at the PL central emission peak from the QDs solution when excited at 450 nm. The amounts of DDT (10 mL) and CuI (0.1 mmol) were held fixed

Cu : In precursor	λ_em/nm	PLQY/%	PL decay/ns
1 : 1	710	3.3	264 (65)
1 : 2	633	8.8	270 (71)
1 : 4	625	18.9	293 (86)
1 : 6	618	21.0	299 (95)

Table S2 Relevant parameters for CuInZnS alloyed QDs synthesized with differnt molar stoichiometric ratios of Cu : In. λem is the PL central emission peak from the QDs solution when excited at 450 nm. The amounts of DDT (10 mL) and CuI (0.1 mmol) were held fixed

Cu : In precursor	λ_em/nm	PLQY/%	PL decay/ns
1 : 1	675	14.7	277 (102)
1 : 2	596	16.8	284 (101)
1 : 4	590	24.8	284 (110)
1 : 6	581	36.3	282 (112)

Table S3 PL lifetime of CuInZnS@ZnS QDs with the stoichiometric ratio of Cu : In at 1 : 2 after excited at 450 nm.

Shell reaction time/h	PL decay/ns
3	588 (204)
5	647 (208)
8	714 (214)
10	724 (211)
12	729 (219)
15	751 (222)
20	755 (231)

Table S4 Relevant parameters for CuInZnS@ZnS QDs with the stoichiometric ratio of Cu : In at 1 : 4, synthesized with different ZnS shell growth time. λem is the PL central emission peak from the QDs solution when excited at 450 nm. The amounts of DDT (10 mL) and CuI (0.1 mmol) were held fixed.

Shell reaction time/h	PL emission peak/nm	PLQY/%	PL decay/ns
5	546	57	509 (171)
10	536	50	530 (177)
15	531	53	558 (174)
20	530	58	549 (165)

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具有可调谐和长寿命荧光发射的高亮度、单分散四元CuInZnS@ZnS量子点

High-brightness and Monodisperse Quaternary CuInZnS@ZnS Quantum Dots with Tunable and Long-lived Emission

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