Zhang Ying^1a， Liu Mingyang^1a， Wang Yihao^1a， Zhang Xiaoli²， Sun Zhiwei^1a， Liu Xiaoyan^1a， Zhou Weijia^1a，1b

——1a.Institute for Advanced Interdisciplinary Research school of Chemistry and Chemical Engineering， 1b.Shandong Key Laboratory of Functional Materials for Integrated Lithium Niobate Photonic， University of Jinan， Jinan 250022， China； 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

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

Get Citation :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

Received : 2026-04-20， Revised ： 2026-06-20，Online ： 2026-08-11。

Funding ： The research was supported by the National Key Research and Development Program of China (Grant No. 2023YFB3210400).

CLC No.: TB34；TB44

Type Code : A

Serial No.: 1008-5548（2026）05-0162-11