Optimization of h-BN/Ag/Ag<sub>2</sub>O heterostructure by high temperature annealing and its surface-enhanced Raman scattering performance

Zheng Lin-Qi; Shi Shu-Hua; Li Jin-Ze; Wang Zi-Yu; Li Shuang

doi:10.7498/aps.72.20231105

Abstract

As a commonly used food additive, synthetic dyes are widely used in foods such as beverages, sweets and dairy products, and in the food processing process. Excessive use of synthetic dyes may induce cell mutations, children’s hyperactivity, genetic diseases and even cancer, which greatly threatens human health. As a fast, cheap, stable, ultra-sensitive and accurate detection method, SERS detection can reflect rich information about molecular fingerprint through the vibration of the analyte, and accurately determine the trace quantity of synthetic dyes in the actual environment. The metal/semiconductor heterostructure formed by the combination of plasmon metal and semiconductor is advantageous for the enhancement of photoinduced charge transfer (PICT) efficiency, and has obvious advantages in the study of surface-enhanced Raman scattering. In this work, the prepared hybrid substrate is annealed to further improve the surface-enhanced Raman scattering activity. Initially, high-density and monodisperse silver/silver oxide (Ag/Ag₂O) nanoparticles are loaded onto two-dimensional hexagonal boron nitride (h-BN) nanosheets. On this basis, by annealing the system at high temperature, an efficient charge transfer channel is constructed, which greatly improves the PICT efficiency and chemical enhancement (CM). It is confirmed experimentally that the SERS signal intensity of h-BN/Ag/Ag₂O material annealed at 320 ℃ with crystal violet (CV) as probe molecule is significantly increased 18 times compared with that of unannealed material, enhancement factor (EF) reaches 16.3145 ×10⁷. Finally, based on the excellent SERS property of h-BN/Ag/Ag₂O annealed at 320 ℃, the SERS detection of food additive Patent Blue V (PBV) is conducted in this work. The results show that the lowest detection concentration can reach 10^–12 M, and the trace detection of synthetic dye PBV is realized. It has excellent spatial uniformity and anti-interference capability, which is of great significance in implementing the actual scene detection of PBV. The h-BN/Ag/Ag₂O annealed at 320 ℃, the composite which is constructed in this paper, has both physical enhancement and chemical enhancement, and possess significant advantages in ultra-low sensitive SERS detection of food additives.

Keywords:

Authors and contacts

School of Science, Shandong Jianzhu University, Jinan 250101, China

Corresponding author: Li Shuang, lishuang@sdjzu.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 11905115).

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References

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Cited By

图 1 (a)—(c) 原始h-BN纳米片, h-BN/Ag/Ag₂O, h-BN/Ag/Ag₂O 320 ℃退火产物的TEM图像(插图为对应纳米材料的溶液); (d), (e) 负载在h-BN上的Ag/Ag₂O纳米颗粒在320 ℃退火前和退火后的粒径分布图

Figure 1. (a)–(c) TEM images of the original h-BN nanosheets, h-BN/Ag/Ag₂O, and h-BN/Ag/Ag₂O annealing products at 320 ℃ (Illustration is the solution of the corresponding nanomaterial); (d), (e) particle size distributions of Ag/Ag₂O nanoparticles loaded on h-BN before and after annealing at 320 ℃.

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图 2 (a) HAADF-STEM图像; (b)—(e) h-BN/Ag/Ag₂O 320 ℃退火复合材料中Ag, O, B和N元素的分布图; (f) 混合后的元素映射图

Figure 2. (a) HAADF-STEM image; (b)–(e) distribution of Ag, O, B and N elements in h-BN/Ag/Ag₂O annealed composite at 320 ℃; (f) mixed element map.

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图 3 h-BN/Ag/Ag₂O 320 ℃退火后的 HRTEM图像(a)和SAED图像(b); 退火前 (c) 和退火后 (d) 的EDS图

Figure 3. HRTEM image (a) and SAED image (b) of h-BN/Ag/Ag₂O after annealed in 320 ℃; EDS image before (c) and after (d) annealed of h-BN/Ag/Ag₂O.

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图 4 (a) 原始h-BN, h-BN/Ag/Ag₂O和h-BN/Ag/Ag₂O 320 ℃退火复合材料的XRD图谱; (b) h-BN/Ag/Ag₂O在不同温度下退火所得产物的紫外-可见光-近红外吸收光谱; (c) h-BN, h-BN/Ag/Ag₂O和h-BN/Ag/Ag₂O 320 ℃退火复合材料的带隙

Figure 4. (a) XRD spectrum of original h-BN nanosheets, h-BN/Ag/Ag₂O and h-BN/Ag/Ag₂O annealed 320 ℃; (b) ultraviolet-visible-near-infrared absorption spectra of materials annealed by h-BN/Ag/Ag₂O at different temperatures; (c) band gaps of h-BN, h-BN/Ag/Ag₂O and h-BN/Ag/Ag₂O annealed at 320 ℃.

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图 5 h-BN, h-BN/Ag/Ag₂O和h-BN/Ag/Ag₂O 320 ℃退火后的光电流响应(a)和 PL光谱(b)

Figure 5. Photocurrent response (a) and PL spectra (b) of h-BN, h-BN/Ag/Ag₂O and h-BN/Ag/Ag₂O after annealed at 320 ℃.

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图 6 (a) 不同退火温度下获得的h-BN/Ag/Ag₂O复合材料作为基底, 对CV (10^–6 M)分子进行拉曼测试得到的SERS光谱, 插图为在320 ℃附近退火后得到的SERS光谱. (b) 不同退火温度的基底对应的CV分子的SERS光谱在1177, 1593, 1621 cm^–1处特征峰的强度分布, 插图为在320 ℃附近退火后的基底所对应的特征峰强度分布

Figure 6. (a) SERS spectrum of CV (10^–6 M) molecules was obtained by Raman test on h-BN/Ag/Ag₂O composites at different annealing temperatures, the inset shows the SERS spectrum obtained after annealing near 320 ℃. (b) Intensity distribution of characteristic peaks of CV molecules corresponding to substrates with different annealing temperatures at 1177, 1593 and 1621 cm^–1, the inset shows the characteristic peak intensity distribution corresponding to the substrate after annealing near 320 ℃.

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图 7 (a) 不同浓度的CV的SERS光谱; (b) CV分子在1621 cm^–1处的SERS强度和分子浓度的对数之间的关系; (c) 不同浓度的R6G的SERS光谱; (d) R6G分子在1502 cm^–1的SERS强度和分子浓度的对数之间的关系

Figure 7. (a) SERS spectra of CV with different concentrations; (b) relationship between SERS intensity and logarithm of molecular concentration of CV molecule at 1621 cm^–1; (c) SERS spectrum of R6G with different concentrations; (d) relationship between SERS intensity and logarithm of molecular concentration of R6G at 1502 cm^–1.

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图 8 (a)不同浓度的PBV的SERS光谱; (b) PBV分子在1619 cm^–1处的SERS强度和分子浓度的对数之间的关系

Figure 8. (a) SERS spectrum of PBV with different concentrations; (b) relationship between SERS intensity and logarithm of molecular concentration of PBV at 1619 cm^–1.

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图 9 (a) 以PBV (10^–6 M)为探针分子, 在h-BN/Ag/Ag₂O 320 ℃退火复合材料上随机选取8个不同位置的点进行检测, 得到的SERS光谱; (b) PBV分子位于1619 cm^–1处的拉曼特征峰强度的变化情况; (c) 在39 μm×39 μm的正方形区域内等距离取得169个点位得到SERS光谱, 峰位在1619 cm^–1处的强度变化情况; (d) 拉曼信号峰位在1619 cm^–1处强度的RSD

Figure 9. (a) Using PBV (10^–6 M) as probe molecule, the SERS spectrum was obtained by randomly selecting 8 points at different positions on the h-BN/Ag/Ag₂O annealed composite at 320 ℃; (b) change of Raman characteristic peak intensity of PBV at 1619 cm^–1; (c) 169 sites were obtained equidistant in a square area of 39 μm×39 μm to obtain SERS spectrum, with the intensity change at 1619 cm^–1; (d) Raman signal peak at 1619 cm^–1 intensity RSD.

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图 10 (a) 浓度为10^–6 M的PBV通过单独添加K⁺, Ca²⁺, Na⁺和Mg²⁺离子(10^–3 M)后的拉曼光谱; (b) 在离子干扰的情况下PBV分子在1619 cm^–1处的拉曼峰强度的波动; (c) 浓度为10^–6 M的PBV与酸奶、气泡水和彩色蛋糕提取液混合的拉曼光谱; (d) 在添加三种干扰物质后1619 cm^–1 处拉曼峰强度的变化

Figure 10. (a) Raman spectra of PBV with a concentration of 10^–6 M by adding K⁺, Ca²⁺, Na⁺ and Mg²⁺ (10^–3 M) alone; (b) the fluctuation of Raman peak intensity of PBV molecule at 1619 cm^–1 in the presence of ion interference; (c) Raman spectra of PBV at a concentration of 10^–6 M mixed with yogurt, sparkling water and colored cake extract; (d) change in Raman peak intensity at 1619 cm^–1 after the addition of three interfering substances.

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Vol. 72, Issue 22 - 2023-11-20

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Optimization of h-BN/Ag/Ag₂O heterostructure by high temperature annealing and its surface-enhanced Raman scattering performance

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Corresponding author: Li Shuang, lishuang@sdjzu.edu.cn

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Optimization of h-BN/Ag/Ag2O heterostructure by high temperature annealing and its surface-enhanced Raman scattering performance

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Corresponding author: Li Shuang, lishuang@sdjzu.edu.cn

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Optimization of h-BN/Ag/Ag₂O heterostructure by high temperature annealing and its surface-enhanced Raman scattering performance