张影^1a， 柳明洋^1a， 王艺洁^1a， 张晓俐²， 孙志伟^1a， 刘晓燕^1a， 周伟家^1a，1b

1.济南大学 a.化学化工学院， 前沿交叉科学研究院， b.山东省铌酸锂光电集成功能材料重点实验室（筹）， 山东 济南 250022；2. Australian Research Council Centre of Excellence for Green Electrochemical Transformation of Carbon Dioxide，Applied Chemistry and Environmental Science， RMIT University， Melbourne， VIC 3001， Australia

引用格式：

张影， 柳明洋， 王艺洁， 等. 激光调控氧掺杂二硫化钼用于降钙素原的拉曼散射检测［J］. 中国粉体技术， 2026， 32（5）： 162-172.

Zhang Ying， Liu Mingyang， Wang Yijie， et al. Laser⁃regulated oxygen⁃doped molybdenum disulfide for SERS detection of procalcitonin［J］. China Powder Science and Technology， 2026， 32（5）： 162-172.

DOI：10.13732/j.issn.1008-5548.2026.05.014

收稿日期： 2026-04-20， 修回日期： 2026-06-20， 上线日期： 2026-08-11。

基金项目： 国家重点研发计划，编号： 2023YFB3210400；

第一作者： 张影（1998—），女，硕士生，研究方向为光信号增强传感基底的构筑及细菌感染标志物检测。E-mail：18654596621@163.com。

通信作者： 周伟家（1982—），男，教授，博士，博士生导师，国家优秀青年科学基金获得者，研究方向为能源催化和功能器件。E-mail：ifc_zhouwj@ujn.edu.cn。

摘要： 【目的】 研究激光热效应调控氧掺杂二硫化钼（oxygen⁃doped molybdenum disulfide，O⁃MoS₂），用于降钙素原（procalcitonin， PCT）的特异性表面增强拉曼散射（surface⁃enhanced Raman scattering， SERS）检测方法。 【方法】 采用激光粗化钼片在表面形成三氧化钼（molybdenum trioxide， MoO₃），经高温气相硫化转化为二硫化钼（molybdenum disulfide，MoS₂），通过改变激光的欠焦距离，利用激光的热效应对MoS₂进行O掺杂的方法制备O⁃MoS₂；调控激光参数实现基底微观形貌、晶格结构调控从而实现SERS增强，以罗丹明6G（rhodamine 6G，R6G）为探针分子评价O⁃MoS₂的SERS性能并对PCT进行检测。 【结果】 O⁃MoS₂基底用于PCT的SERS检测具有稳定性和特异性，对PCT的检测限为0.45 μg·mL^-1。 【结论】 激光热效应法可实现O原子在MoS₂中的均匀掺杂，O掺杂能显著增强MoS₂的SERS性能，O⁃MoS₂基底检测具有较好的稳定性与特异性，为非贵金属SERS基底制备提供新路径，可用于细菌感染相关生物标志物检测。

关键词： 表面增强拉曼散射； 激光热效应； 氧掺杂二硫化钼； 降钙素原

Abstract

Objective To address the issues of high cost and poor stability of noble metal surface⁃enhanced Raman scattering（SERS） substrates， as well as insufficient active sites and low charge transfer efficiency of pure MoS₂， the laser thermal effect is used to achieve controllable oxygen doping of MoS₂， to prepare a highly uniform O-MoS₂ SERS substrate， and to establish a specific SERS detection method for the bacterial infection biomarker procalcitonin （PCT）.

Methods High-purity molybdenum sheets were used as raw materials and etched by a 1 064 nm pulsed laser in air to form MoO₃. Using 10 vol% H₂S as the sulfur source， the MoO₃ was sulfurized at high temperature to obtain pure-phase MoS₂. Oxygen doping of MoS₂ was carried out in air using defocused laser irradiation to obtain O-MoS₂. The phase， morphology， crystal structure， surface chemical state， and SERS performance of the materials were characterized and tested using XRD， SEM， HRTEM， XPS， and laser confocal Raman spectroscopy. Using rhodamine 6G （R6G） as the SERS probe molecule， the laser power and number of laser irradiation cycles for oxygen doping were optimized， and the O-MoS₂ with optimal SERS performance was used for PCT detection.

Results and Discussion When the laser defocus distance was 6 cm， the temperature on the MoS₂ surface was 324 ℃， which satisfied the conditions required for oxygen doping. Oxygen doping did not destroy the crystal structure of MoS₂ but only caused slight lattice distortion， which was beneficial for ion transport and provided more active sites. The optimal SERS performance of the O-MoS₂ substrate was achieved at a laser power of 3% and one irradiation cycle， under which the oxygen doping amount on the material surface was the highest. The Raman signal of O-MoS₂ was about 10 times higher than that of MoS₂. Characteristic peaks were still observed at an R6G concentration of 10⁻⁷ mol·L， and the relative standard deviations of the characteristic peak signals at 10 test sites were all <5%， indicating excellent detection repeatability and stability. When applied to PCT detection， the characteristic peak intensity of PCT showed a good linear relationship with the concentration in the range of 1-30 mg·L^-1. The linear equation was y = 2 425.04+559.50x， R² =0.977 01， and the limit of detection was 0.45 mg·L^-1. Specificity experiments showed that IL-6 and CRP caused almost no interference， indicating that the O-MoS₂ substrate exhibited specificity for PCT detection.

Conclusion 1） To address the issues of poor doping uniformity and uncontrolled distribution of oxygen active sites in conventional O-MoS₂ preparation methods， a strategy based on the laser thermal effect is proposed for site-specific oxygen doping regulation of the MoS₂ substrate， which enables uniform doping of O atoms in the MoS₂ substrate. 2） The O-MoS₂ substrate prepared by laser-thermal-effect regulation exhibits excellent SERS performance and surface stability. Using R6G as the probe molecule， the lower limit of signal response reaches 10⁻⁷ mol·L， and the relative standard deviations of the characteristic peaks at 10 test sites on the same substrate are all less than 5%， demonstrating good detection repeatability and stability. 3） When applied to PCT detection， it shows a good linear relationship between concentration and Raman signal intensity in the target concentration range of 1~30 mg·L⁻¹， with a detection limit of 0.45 mg·L⁻¹. This study provides a high-performance substrate material and a preparation method for the SERS detection of biomarkers.

Keywords： surface-enhanced Raman scattering； laser thermal effect； oxygen-doped molybdenum disulfide； procalcitonin

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