Improvement of SERS detection performance based on MoS<sub>2</sub>/Zeolitic imidazolate framework-67 heterostructure

LI Binjiang; ZHANG Yuchen; LI Wei; WANG Xuehua

doi:10.7498/aps.74.20250410

Abstract

Earth-abundant molybdenum disulfide (MoS₂), as a promising substrate for surface-enhanced Raman spectroscopy (SERS), has attracted considerable attention. Naturally occurring MoS₂ primarily exists in the semiconducting 2H phase, but its SERS performance is limited because active sites are typically confined to its edges. Furthermore, the irregular agglomeration of MoS₂ can lead to performance degradation, making natural semiconducting material unsuitable for practical applications. Therefore, enhancing the performance of MoS₂ in the field of SERS is of great significance. Metal-organic frameworks (MOFs) are ideal materials for building efficient SERS substrates due to their tunable pore structures. Among various MOF materials, zeolitic imidazolate frameworks (ZIFs) have aroused significant interest due to their well-defined polyhedral structures, homogeneity, and small particle sizes. Therefore, in this study, MoS₂/zeolitic imidazolate framework-67 (ZIF-67) heterostructures are prepared by the hydrothermal method as SERS substrates, which exhibits exceptionaly high sensitivity to rhodamine 6G with an enhancement factor of up to 6.68×10⁶. Moreover, after SERS is exposed to air for four months, its performance remains almost unchanged, demonstrating high stability and reusability. To evaluate the actual detection ability of this substrate, bilirubin is selected as the analyte, which is a clinically relevant metabolic waste. Since both high and low concentrations of free bilirubin can lead to cardiovascular and cerebrovascular diseases, accurate monitoring of bilirubin levels is crucial for diagnosing bilirubin-induced disorders. Using the MoS₂/ZIF-67 substrate, the label-free detection of bilirubin is achieved with a limit of detection as low as 10^–10 mol/L. The outstanding performance of this substrate can be attributed to the vertically aligned MoS₂ nanostructure, which exposes more active sites. Additionally, ZIF-67 provides a high specific surface area and abundant porous structures, providing numerous adsorption sites for target molecules. Furthermore, the internal charge transfer facilitates the formation of a highly conductive 1T phase, thereby improving electrical conductivity. This work provides valuable insights into the rational designing of noble-metal-free materials for highly sensitive SERS detection.

Keywords:

Authors and contacts

State Key Laboratory of Optoelectronic Materials and Technologies, School of Physics, Sun Yat-sen University, Guangzhou 510275, China

Corresponding author: WANG Xuehua, wangxueh@mail.sysu.edu.cn

Funds: Project supported by the National Natural Science Foundations of China (Grant Nos. 12334017, 12374326) and the National Key R&D Program of China (Grant No. 2021YFA1400800).

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References

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Cited By

图 1 ZIF-67, MoS₂和xMoS₂/ZIF-67的合成流程示意图

Figure 1. Schematic diagram of the synthesis of ZIF-67, MoS₂ and xMoS₂/ZIF-67.

DownLoad: Full-Size Img PowerPoint

图 2 MoS₂, ZIF-67和MoS₂/ZIF-67的(a) XRD图、(b)拉曼光谱和(c)傅里叶变换红外光谱

Figure 2. (a) XRD patterns, (b) Raman spectra, and (c) FT-IR spectra of MoS₂, ZIF-67 and MoS₂/ZIF-67.

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图 3 基底的SEM, TEM和EDS图　(a) MoS₂, (b) ZIF-67和(c) 0.3MoS₂/ZIF-67的SEM图像; (d) MoS₂, (e) ZIF-67和(f) 0.3MoS₂/ZIF-67的TEM图像; (g) 0.3MoS₂/ZIF-67的HRTEM; (h) 图(g)中蓝色矩形区域放大后的图片; (i)—(l) Co, Mo, S, O的EDS元素映射图

Figure 3. SEM images of (a) MoS₂, (b) ZIF-67 and (c) 0.3MoS₂/ZIF-67; TEM images of (d) MoS₂, (e) ZIF-67 and (f) 0.3MoS₂/ZIF-67; (g) HRTEM of 0.3MoS₂/ZIF-67; (h) magnified domains of the blue rectangle; (i)–(l) EDS element mapping images of Co, Mo, S and O.

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图 4 基底的XPS图　(a), (c), (d) MoS₂和0.3MoS₂/ZIF-67的(a) Mo 3d谱、(c) S 2p谱和(d) O 1s谱; (b) ZIF-67和0.3MoS₂/ZIF-67的Co 2p谱

Figure 4. (a) Mo 3d spectrum, (c) S 2p spectrum and (d) O 1s spectrum of MoS₂ and 0.3MoS₂/ZIF-67; (b) Co 2p spectrum of ZIF-67 and 0.3MoS₂/ZIF-67.

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图 5 基底的拉曼光谱和SERS性能图　(a) R6G(10^–3 mol/L)吸附在MoS₂, ZIF-67和xMoS₂/ZIF-67上的SERS谱图; (b) 0.3MoS₂/ZIF-67基底上不同浓度R6G的SERS光谱; (c) 1653 cm^–1处SERS强度与对数浓度的线性关系; (d) 0.3MoS₂/ZIF-67的可重复性、(e)循环性和(f)稳定性表征

Figure 5. (a) SERS spectra of R6G (10^–3 mol/L) adsorbed on MoS₂, ZIF-67 and xMoS₂/ZIF-67; (b) SERS spectra of R6G of various concentrations enhanced by 0.3MoS₂/ZIF-67; (c) linear relationship of SERS intensities at 1653 cm^–1 versus logarithm of concentration; (d) reproducibility, (e) cyclicity and (f) stability of 0.3MoS₂/ZIF-67.

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图 6 R6G-0.3MoS₂/ZIF-67的能级和电荷转移示意图

Figure 6. Diagram of the energy level and charge transfer in the R6G-0.3MoS₂/ZIF-67.

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图 7 复合后的基底与非复合基底的SERS性能对比图　(a)不同浓度胆红素在0.3MoS₂/ZIF-67基底上的SERS光谱和(b) 1614 cm^–1处信号强度与胆红素对数浓度的关系; (c)不同浓度胆红素在MoS₂基底上的SERS光谱和(d) 1614 cm^–1处信号强度与胆红素对数浓度的关系

Figure 7. SERS spectra of (a) 0.3MoS₂/ZIF-67 and (c) MoS₂ substrates with various concentrations of bilirubin. Plot of the intensity at 1614 cm^–1 against the logarithmic concentration of bilirubin in the presence of (b) 0.3MoS₂/ZIF-67 and (d) MoS₂.

DownLoad: Full-Size Img PowerPoint

[1]	Odum E P 1969 Science 164 262 Google Scholar
[2]	Guo Y, Liu Y 2022 J. Geog. Sci. 32 23 Google Scholar
[3]	Zhang Y, Gao F, Wang D, Li Z, Wang X, Wang C, Zhang K, Du Y 2023 Coord. Chem. Rev. 475 214916 Google Scholar
[4]	Li Y, Zhang J, Chen Q, Xia X, Chen M 2021 Adv. Mater. 33 2100855 Google Scholar
[5]	Hou H, Anichini C, Samorì P, Criado A, Prato M 2022 Adv. Funct. Mater. 32 2207065 Google Scholar
[6]	Li J, Chen C, Lv Z, Ma W, Wang M, Li Q, Dang J 2023 J. Mater. Sci. Technol. 145 74 Google Scholar
[7]	Gong C, Li W, Lei Y, He X, Chen H, Du X, Fang W, Wang D, Zhao L 2022 Composites Part B 236 109823 Google Scholar
[8]	Reyren N, Thiel S, Caviglia A D, Kourkoutis L F, Hammerl G, Richter C, Schneider C W, Kopp T, Rüetschi A S, Jaccard D, Gabay M, Muller D A, Triscone J-M, Mannhart J 2007 Science 317 1196 Google Scholar
[9]	Ohtomo A, Hwang H Y 2004 Nature 427 423 Google Scholar
[10]	Chen W, Zhu X, Wang R, Wei W, Liu M, Dong S, Ostrikov K K, Zang S Q 2022 J. Energy Chem. 75 16 Google Scholar
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[12]	Wang H, Niu Z, Peng Z, Wu X, Gao C, Zhao S, Kim Y D, Wu H, Du X, Liu Z, Li B 2022 ACS Appl. Mater. Interfaces 14 9116 Google Scholar
[13]	Xu H, Zhu J, Ma Q, Ma J, Bai H, Chen L, Mu S 2021 Micromachines 12 240 Google Scholar
[14]	Cao Y 2021 ACS Nano 15 11014 Google Scholar
[15]	He H, Li X, Huang D, Luan J, Liu S, Pang W K, Sun D, Tang Y, Zhou W, He L, Zhang C, Wang H, Guo Z 2021 ACS Nano 15 8896 Google Scholar
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[23]	Quan Y, Li J, Hu M, Wei M, Yang J, Gao M, Liu Y 2022 Appl. Surf. Sci. 598 153750 Google Scholar
[24]	Li M, Cai B, Tian R, Yu X, Breese M B H, Chu X, Han Z, Li S, Joshi R, Vinu A, Wan T, Ao Z, Yi J, Chu D 2021 Chem. Eng. J. 409 128158 Google Scholar
[25]	Xu J, Cheng C, Shang S, Gao W, Zeng P, Jiang S 2020 ACS Appl. Mater. Interfaces 12 49452 Google Scholar
[26]	Li Q, Huang F, Li S, Zhang H, Yu X 2022 Small 18 2104323 Google Scholar
[27]	Sundara Venkatesh P, Kannan N, Ganesh Babu M, Paulraj G, Jeganathan K 2022 Int. J. Hydrogen Energy 47 37256 Google Scholar
[28]	Xu J, Shang S, Gao W, Zeng P, Jiang S 2021 Cellulose 28 7389 Google Scholar
[29]	Chen Y, Meng G, Yang T, Chen C, Chang Z, Kong F, Tian H, Cui X, Hou X, Shi J 2022 Chem. Eng. J. 450 138157 Google Scholar
[30]	Rafiei S, Tangestaninejad S, Horcajada P, Moghadam M, Mirkhani V, Mohammadpoor-Baltork I, Kardanpour R, Zadehahmadi F 2018 Chem. Eng. J. 334 1233 Google Scholar
[31]	Chang J, Wang Y, Chen L, Wu D, Xu F, Bai Z, Jiang K, Gao Z 2020 Int. J. Hydrogen Energy 45 12787 Google Scholar
[32]	Hou B, Wu J 2020 Dalton Trans. 49 17621 Google Scholar
[33]	Leng X, Wang Y, Wang F 2019 Adv. Mater. Interfaces 6 1900010 Google Scholar
[34]	Mohammadpour E, Asadpour-Zeynali K 2020 Microchem J. 157 104939 Google Scholar
[35]	Hou X, Zhou H, Zhao M, Cai Y, Wei Q 2020 ACS Sustainable Chem. Eng. 8 5724 Google Scholar
[36]	Liu Z, Gao Z, Liu Y, Xia M, Wang R, Li N 2017 ACS Appl. Mater. Interfaces 9 25291 Google Scholar
[37]	Li X, Lü X, Li N, Wu J, Zheng Y Z, Tao X 2019 Appl. Catal., B 243 76 Google Scholar
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[43]	Nguyen D C, Tran D T, Doan T L L, Kim D H, Kim N H, Lee J H 2020 Adv. Energy Mater. 10 1903289 Google Scholar
[44]	Zhu H, Zhang J, Yanzhang R, Du M, Wang Q, Gao G, Wu J, Wu G, Zhang M, Liu B, Yao J, Zhang X 2015 Adv. Mater. 27 4752 Google Scholar
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[46]	Ganesan P, Sivanantham A, Shanmugam S 2018 J. Mater. Chem. A 6 1075 Google Scholar
[47]	Li W, Liu J, Guo P, Li H, Fei B, Guo Y, Pan H, Sun D, Fang F, Wu R 2021 Adv. Energy Mater. 11 2102134 Google Scholar
[48]	Sun H, Yao M, Song Y, Zhu L, Dong J, Liu R, Li P, Zhao B, Liu B 2019 Nanoscale 11 21493 Google Scholar
[49]	Wang X, Han Y, Liu Y, Yu Y, Ma J, Yang T, Hu J, Huang H 2023 Int. J. Hydrogen Energy 48 3048 Google Scholar
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[52]	Gupta J D, Jangra P, Mishra A K 2025 ACS Appl. Nano Mater. 8 7449 Google Scholar
[53]	Lombardi J R, Birke R L 2014 J. Phys. Chem. C 118 11120 Google Scholar

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[20]	Wu Mu-Sheng, Xu Bo, Liu Gang, Ouyang Chu-Ying. The effect of strain on band structure of single-layer MoS2: an ab initio study. Acta Physica Sinica, 2012, 61(22): 227102. doi: 10.7498/aps.61.227102

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Vol. 74, Issue 12 - 2025-06-20

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Improvement of SERS detection performance based on MoS₂/Zeolitic imidazolate framework-67 heterostructure

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Corresponding author: WANG Xuehua, wangxueh@mail.sysu.edu.cn

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Improvement of SERS detection performance based on MoS2/Zeolitic imidazolate framework-67 heterostructure

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Improvement of SERS detection performance based on MoS₂/Zeolitic imidazolate framework-67 heterostructure