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. 2025 Aug 1;15:28087. doi: 10.1038/s41598-025-12193-2

Localized surface plasmon resonance sensing of hydrogen sulfide using zinc oxide film

Yuki Takimoto 1,✉, Keiji Komatsu 2, Hiromasa Namiki 1, Kazuto Mochizuki 1, Tomoe Nakagawa 1, Kohki Nagata 1, Kazuki Komiya 1, Tomoko Gessei 1, Akira Monkawa 1
PMCID: PMC12317021  PMID: 40750806

Abstract

A localized surface plasmon resonance (LSPR) sensor for hydrogen sulfide (H2S) has been developed by coating a gold nanopattern with zinc oxide (ZnO) film. H2S detection was achieved by monitoring changes in absorbance at a specific wavelength in the LSPR spectrum. The absorbance increased during exposure to H2S and remained constant after H2S ceased. These responses indicate that the sensor can measure the integrated concentrations of H2S. The sensitivity to H2S was enhanced with increasing relative humidity, enabling detection of 0.05–3 ppm H2S within 10 min at 70% relative humidity. The sensor’s sensitivity and LSPR spectrum could be restored by heating it at 500 °C in air. Notably, the sensor did not respond to methyl mercaptan or dimethyl sulfide, demonstrating high selectivity for H2S. This study highlights the potential of the ZnO-deposited LSPR sensor for highly sensitive and selective detection of H2S.

Supplementary Information

The online version contains supplementary material available at 10.1038/s41598-025-12193-2.

Keywords: Localized surface plasmon resonance (LSPR), Au nanopattern, Zinc oxide, Hydrogen sulfide, Volatile sulfur compounds (VSCs), Periodontal disease

Subject terms: Imaging and sensing, Nanoparticles

Introduction

Oral hygiene management is crucial for maintaining oral health, which contributes significantly to an individual’s quality of life (QOL) and healthy life expectancy1. However, oral diseases are widespread worldwide and greatly reduce the QOL of those affected2. For example, more than half of the global population suffers from periodontal disease, underscoring the growing importance of prevention. Many studies have reported that halitosis, or bad breath, is closely related with oral diseases such as periodontal disease3–5. Halitosis not only causes discomfort but also leads to social embarrassment6. Thus, halitosis testing is an effective oral hygiene technique for maintaining a good QOL. The primary causative agents of halitosis are volatile sulfur compounds (VSCs) produced by bacteria in the oral cavity7–9. The key VSCs include hydrogen sulfide (H2S), methyl mercaptan (CH3SH), and dimethyl sulfide ((CH3)2S). Studies have reported that the concentrations of H2S and CH3SH in oral diseases are typically at the sub-ppm order, with variations depending on the specific type of oral disease10. Therefore, monitoring VSCs with high sensitivity and selectivity is essential for effective oral hygiene management.

Conventional methods for measuring VSCs in clinical practice include organoleptic examination, electrochemical sensors, and gas chromatography (GC-MS). Organoleptic examination is a simple method in which a breath assessor rates halitosis on a scale of 0 to 511. However, this method has several drawbacks, such as subjective evaluation, low reproducibility, the need for trained evaluators, and the risk of disease transmission. Electrochemical sensors can measure the concentration of H2S and CH3SH at the ppb level3,6,12. Although these sensors are easy to use, portable, and inexpensive, they cannot distinguish between the concentrations of different VSCs, and their readings can be affected by interference from other volatile organic compounds (VOCs) such as acetone and ethanol. Conventional GC-MS systems equipped with a flame photometric detector can measure three VSCs13,14. However, this technique requires expensive, large equipment and trained operators who must perform complicated procedures. A portable GC-MS has been developed to address these limitations4,13. This device can distinguish between the three VSCs with high sensitivity, is easy to handle, and is relatively inexpensive. Although clinical testing devices have become smaller and simpler, they are still too expensive and large for individuals to use for daily oral hygiene monitoring. Therefore, a smaller, less expensive sensor with high sensitivity and selectivity is needed.

In recent years, localized surface plasmon resonance (LSPR) has been applied to the production of useful substances by photocatalysis and the sensing of various materials such as proteins, VOCs, and inorganic gas molecules15–21. LSPR is the phenomenon in which conduction electrons on the surface of a metallic nanostructure collectively vibrate in resonance with light, resulting in absorption at a specific wavelength22. The absorption wavelength varies depending on the metal species (Au, Ag, Cu etc.), nanostructure, and the refractive index (RI) around the metal nanostructure. Target molecules are detected by changes in RI and the corresponding shift in the absorption wavelength induced by their approach to the metal nanostructures. To enhance sensitivity, metal nanostructures are often decorated with substances that interact with the target molecules. These nanostructures can be fabricated using cost-effective methods such as nanoimprint lithography and nanosphere lithography23–26. As a result, LSPR sensors are attracting attention as compact and inexpensive devices capable of detecting a wide range of substances with high sensitivity.

There are still few reports on LSPR sensors for detecting H2S. For example, Au nanoparticles dispersed in TiO2–NiO thin films have been reported to detect 2–10 ppm H2S at 350 °C via catalytic oxidation of H2S to SO227. Another study demonstrated that a monolayer film of self-assembled Ag nanoparticles could detect 1–100 ppm H2S in N2 at 25 °C by monitoring changes in the LSPR absorption wavelength caused by Ag2S formation28. In our previous study, an Au nanopattern coated with ZIF-8, one of metal organic frameworks, was able to detect 0.1–20 ppm SO2 and 0.1–10 ppm H2S at 70% relative humidity (RH) and 25°C29. Despite the relatively high sensitivity of this sensor, ZIF-8 degraded over time when exposed to H2S and SO2, leading to reduced sensitivity. Furthermore, the sensor also responded to changes in RH due to water absorption by the porous nature of ZIF-8.

Zinc oxide (ZnO) has been widely used as a versatile functional material, serving both as a sensing material for various gases, including H2S, and as an adsorbent for the desulfurization of factory exhaust gases30–33. Semiconductor sensors employing ZnO have been shown to detect H2S in the sub-ppm to ppm range at operating temperatures between room temperature and 300°C34,35. ZnO reacts with H2S to form ZnS, a reactivity that has been leveraged in surface plasmon resonance (SPR) sensors. These sensors, using optical fibers, have been developed for the detection of 10–100 ppm H2S in N2 at room temperature31,36–38. These sensors were fabricated by coating ZnO and Cu or Ag layers onto the unclad portions of optical fibers. The characteristics of ZnO make it a promising candidate for application in LSPR sensors. Unlike porous materials, non-porous ZnO does not absorb water, even under high humidity conditions, which minimizes water-induced responses. Additionally, ZnO-coated LSPR sensors can be regenerated by heating after H2S measurement, as ZnS can be oxidized back to ZnO in air at 500 °C or higher39. Therefore, in this study, LSPR sensors for H2S detection were developed by depositing ZnO onto the surface of Au nanopatterns. The effects of RH on sensor sensitivity, the reusability of the sensors following heating, and their selectivity for H2S over CH3SH and (CH3)2S were thoroughly investigated.

Results and discussion

Characteristics of ZnO-deposited LSPR sensors and their response to H2S

 ZnO-deposited LSPR sensors were fabricated by chemical vapor deposition of a 30 nm thick ZnO layer onto an Au nanopattern with a diameter of 650 nm, a pitch of 1000 nm, and a height of 120 nm, on a SiO2 glass substrate (Fig. 1 and S1). The thickness of the ZnO layer was estimated based on the deposition rate. ZnO uniformly and thinly coated the Au nanopattern, as shown in Fig. 1. The refraction peaks of ZnO and Au were observed by X-ray diffraction measurement (Fig. S2). Our previous simulation results revealed that the sensitivity of the Au nanopattern with the LSPR absorbance spectrum in the near-infrared (NIR) region was higher than in the visible region40. In addition, Au is more durable to the corrosive H2S than Ag or Cu. Therefore, the Au nanopattern showing LSPR in the NIR region was also used in this study for the highly sensitive detection of H2S (Fig. 2a).

Fig. 1.

Fig. 1

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(a) SEM image of a ZnO-deposited Au nanopattern on a SiO2 glass substrate. SEM-EDS elemental mapping showing the (b) Au, (c) Zn and (d) O distribution.

Fig. 2.

Fig. 2

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(a) Localized surface plasmon resonance (LSPR) spectra of a ZnO-deposited sensor before (blue line) and after exposure to 3 ppm H2S gas at 70% RH for 10 min (red line). The black dashed line indicates the position of the inflection point where the absorbance change was measured. The wavelength in this spectrum was approximately 1285 nm. (b) Absorbance changes of the ZnO-deposited sensor induced by 3 ppm H2S from 5 to 15 min at 70% RH.

The LSPR absorbance spectra of the sensors exhibited a shift to higher wavelengths upon exposure to H2S gas. For instance, Fig. 2a shows the LSPR spectra of a sensor before and after exposure to 3 ppm H2S for 10 min at 70% RH. This shift indicates an increase in the RI surrounding the Au nanopattern, changing from ZnO (n = 1.57 at 1285 nm) to ZnS (n = 2.28 at 1285 nm)41. Approximately 30 sensors were used to assess sensor performance. The LSPR spectra of these sensors varied slightly; the average peak wavelength and absorbance were 1472 ± 18 nm and 1.10 ± 0.17, respectively. Wavelengths associated with maximum absorbance changes due to H2S exposure also varied depending on spectral differences and H2S concentration. To standardize measurements, absorbance changes were measured at the inflection point of each sensor’s spectrum before exposure, rather than at the wavelength showing the largest absorbance change. This approach facilitates the use of portable, low-cost sensors, as absorbance can be measured using a photodiode and band-pass filter instead of a more expensive spectrometer.

Figure 2b illustrates the absorbance change of a sensor induced by 3 ppm H2S exposure for 10 min at 70% RH, at approximately 1285 nm. For clarity, decreases in absorbance caused by H2S exposure were treated as positive values. The absorbance increased almost linearly during H2S exposure as ZnO reacted with H2S to form ZnS. Since ZnS does not oxidize back to ZnO at room temperature, the absorbance remained stable even after H2S exposure ceased. Consequently, the sensor can provide integrated H2S concentrations, similar to gas detector tubes.

Effect of RH on sensitivity

 The absorbance remained relatively unchanged across RH levels from < 1–70% in the absence of H2S (Fig. S3). Minor variations in absorbance could be attributed to water adsorption on the ZnO film surface. By contrast, LSPR sensors coated with the porous material (ZIF-8) in our previous study exhibited significant RH sensitivity, with absorbance changes comparable to those induced by 10 ppm H2S at 70% RH29. These results highlight the non-porous nature of ZnO films which has the benefit of suppressing absorbance changes due to H2O itself. Exhaled breath typically contains RH levels ranging from 42 to 91%, making the films’ nature advantageous for practical H2S measurements in moist conditions42.

Figure 3 shows the absorbance changes induced by 1 ppm H2S at RH levels from < 1–70%. The absorbance increased with RH and was approximately 18 times greater at 70% RH compared to < 1% RH. This observation indicates that water enhanced the reaction between ZnO and H2S. This result is consistent with Zhao et al.’s report on the increased H2S capacity of ZnO adsorbents in the presence of water43. The proposed mechanism is as follows: hydroxyl groups derived from H2O on the ZnO surface modify the reaction process and lower the reaction activation energy, thereby enhancing ZnO activity. On the other hand, at very high humidity, the activity of ZnO is adversely reduced by H2O43. It is possible that the sensitivity of the sensors may decrease at humidities above 70% RH. The sensitivity above 70% RH could not be verified because of the limitation of this experimental system. The high sensitivity under high humidity (at least 70% RH) is also advantageous for practical measurements, although it is necessary to account for the effect of RH on absorbance changes.

Fig. 3.

Fig. 3

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Absorbance changes induced by 1 ppm H2S exposure versus relative humidity (n = 3).

Regeneration of the sensors

 ZnS is oxidized to ZnO when heated above 500 °C in air39. Therefore, after exposure to H2S, the ZnO-deposited sensors were heated at 500 °C in air for 1 h to regenerate them. The absorbance changes remained nearly constant from the first to the third regeneration cycles (Fig. 4a). This indicates that the sensor can be reused multiple times through a heat regeneration process. The large error bars were attributed to variations in the sensitivity of individual sensors, which could be improved by ensuring consistent sensor quality. In addition, the deviation became larger because the absorbance changed more significantly with a higher concentration of H2S. For the initial regeneration (i.e., the first use of the sensors), the absorbance changes for 2 and 3 ppm H2S were smaller than those after the first to third regenerations. This may be due to the reaction of ZnO with 2–3 ppm H2S and the oxidation of ZnS, which could cause deformation or cracking of the ZnO film, increasing its surface area and enhancing reactivity. However, no significant difference in the film’s morphology was observed.

Fig. 4.

Fig. 4

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(a) Absorbance changes induced by 0.05, 0.5, 1, 2, and 3 ppm H2S exposure for 10 min after each regeneration treatment (heat at 500 °C in air for 1 h after H2S exposure) (n = 3). At the initial regeneration the sensors were not heated and were used for the first time. (b) LSPR spectra of a ZnO-deposited sensor unused (black line), after the 1 st (blue line), the 2nd (red line), and the 3rd regeneration treatment (green line).

After the first two regenerations, the LSPR spectra showed reduced absorbance and a 10 nm peak shift (Fig. 4b). This result suggests deformation of the ZnO film and/or partial integration of unoxidized ZnS. By the third regeneration, the spectra stabilized and were nearly identical to those from the second regeneration, indicating that the film reached a steady state and that the sensors could be reused reliably.

Calibration curve at 70% RH

 The responses to 0.05–2 ppm H2S at 70% RH after the third regeneration followed a comparable trend of 3 ppm H2S (Fig. 5a). Figure 5b shows the linear calibration curve for H2S concentrations ranging from 0.05 ppm to 3 ppm at 70% RH after the third regeneration. The sensitivity obtained from the slope of the calibration curve was 0.00914 ppm−1. The limit of detection (LOD, 3σ) was 0.02 ppm, comparable to that of commercial electrochemical sensors used in clinical practice. The LOD was below the odor recognition threshold for H2S (0.02–0.13 ppm), enabling the sensor to detect H2S in exhaled breath at concentrations reported for periodontal disease patients (~ 0.1 ppm)10,44. Longer exposure times could allow detection of even lower concentrations as the sensor obtains integrated concentration. Furthermore, the sensor’s applicability extends beyond oral hygiene, making it suitable for monitoring H2S emissions from industrial and natural sources such as factories and volcanoes45.

Fig. 5.

Fig. 5

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(a) Absorbance changes induced by 0.05, 0.5, 1, 2, and 3 ppm H2S from 5 to 15 min at 70% RH. (b) Absorbance changes versus the concentrations of H2S at 70% RH after the third regeneration treatment (n = 3).

Selectivity to H2S

 The sensors were exposed to 2 ppm of CH3SH and (CH3)2S, representative VSCs present in exhalation alongside H2S, at 70% RH and were barely detected, as shown in Fig. 6. The absorbance change for H2S was approximately 177 and 365 times larger than those for CH3SH and (CH3)2S, respectively, demonstrating the high selectivity of the sensors for H2S. Although CH3SH and (CH3)2S can adsorb onto the surface of ZnO with Zn-S bonding, the adsorption amounts appeared too small to cause significant changes in the RI around the Au nanopattern46,47. Similarly, these sensors are unlikely to respond to other VOCs that neither react with nor adsorb significantly onto ZnO. On the other hand, LSPR sensors coated with mesoporous silica, as developed in our previous study, could detect a variety of VOCs due to the non-selective absorption capability of porous materials48. By contrast, the ZnO film lacks such absorption capabilities due to its non-porous nature. This selective chemical reactivity and absence of absorption in ZnO films contributes to its high selectivity for H2S. Therefore, the ZnO-deposited sensor demonstrates excellent potential for selectively detecting H2S in exhaled air containing various VOCs. In the future, LSPR sensors for CH3SH and (CH3)2S could be developed by fabricating selective films that specifically react with these compounds. Highly selective VSC sensors would be invaluable for diagnosing and identifying various oral diseases.

Fig. 6.

Fig. 6

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Absorbance changes induced by 10-min exposure to 2 ppm H2S, CH3SH, and (CH3)2S at 70% RH.

Conclusions

An LSPR sensor for highly sensitive and selective detection of H2S was developed by depositing ZnO onto an Au nanopattern on a glass substrate. The sensor exhibited a linear increase in absorbance during H2S exposure, which remained stable after exposure ceased, enabling the measurement of the integrated H2S concentration. Sensitivity was enhanced with increasing humidity; at 70% RH, the sensor detected 0.05–3 ppm H2S within 10 min. In contrast, CH3SH and (CH3)2S were not detected, underscoring the sensor’s high selectivity. The sensitivity was nearly fully recovered after H2S exposure by heating the sensors at 500 °C in air, allowing repeated use for at least three cycles. Thus, the developed sensor shows strong potential for applications in monitoring H2S in exhaled breath and other settings. In the future, applications for measuring other gases such as SO2 will be investigated because the sensor can have the ability to detect gases that react with ZnO.

Methods

Fabrication of a ZnO-deposited LSPR sensor

 An Au nanopattern was fabricated on a SiO2 glass substrate (10 mm × 10 mm × 1 mm) in collaboration with Kyodo International, Inc (Kanagawa, Japan). The metal coating process was conducted using a sputtering machine (EIS-230; Elionix Inc., Tokyo, Japan), with a 20 nm Si adhesion layer between the Au nanopattern and the SiO2 glass substrate. Additional processes, such as nanoimprinting, were also carried out by Kyodo International, Inc. After the substrate was heated at 450 °C for 1 h, a 30 nm thick ZnO layer was deposited onto the Au nanopattern via chemical vapor deposition. The reactant, bis(dipivaloylmethanato)zinc (Zn(DPM)2, Kojundo Chemical Laboratory Co., Ltd., Saitama, Japan), was vaporized using an electric heater. The reactant vapor was carried by nitrogen gas flowing at a rate of 1.5 L/min and sprayed directly onto the substrates mounted on an electric heater. The distance between the nozzle and the substrate was kept at 25 mm. Vaporizer (Tv) and substrate (Ts) temperatures were measured using K-type thermocouples and maintained at 120 and 400 oC, respectively. Surface topography was analyzed using an atomic force microscope (AFM, SPM-9700HT; Shimadzu Corp., Kyoto, Japan) and a field emission scanning electron microscope (FE-SEM, SU-8600; Hitachi High-Tech Corp., Tokyo, Japan). The X-ray diffraction pattern was obtained with an X-ray diffractometer (SmartLab SE; Rigaku Corp., Tokyo, Japan).

Gas detection experiments

 The gas-sensing system used for this study was described in detail in our previous work29. Air containing 0.05–3 ppm H2S, 2 ppm CH3SH, or 2 ppm (CH3)2S was generated using the permeation-tube method. During the 20-min measurement period, background air flowed continuously, with air containing the target gas introduced from 5 to 15 min at a controlled flow rate of 500 mL/min (MQV 9500; Azbil Corp., Tokyo, Japan). The exposure time to the target gas (10 min) was chosen to detect 0.05 ppm H2S at 70% RH. The RH of the air was controlled from < 1–70% by mixing dry air (RH < 1%) with saturated water vapor. 70% RH was the maximum value in this system. LSPR absorbance spectra were measured using a tungsten halogen lamp (HL-2000; Ocean Optics Inc., Largo, FL, USA) and a near-infrared spectrometer (NIRQuest; Ocean Optics Inc.) connected to the sensing chamber via optical fibers. Sensor responses were recorded as absorbance changes at a fixed wavelength, determined from the inflection point of the pre-exposure LSPR spectrum. The experiments were conducted at room temperature (25 °C). After exposure to air containing H2S, sensors were regenerated by heating at 500 °C in air for 1 h to oxidize ZnS back to ZnO.

Supplementary Information

Below is the link to the electronic supplementary material.

Supplementary material 1 (PDF 289.1 kb) (289.1KB, pdf)

Author contributions

Y.T. and K.K. designed the methodology, collected data, analyzed the results, and wrote and revised the manuscript. H.N. collected XRD data. K.M., T.N., K.N. and K.K. helped in LSPR sensing experiments and data analysis. T.G. and A.M. supervised the entire research project. All authors discussed and commented on the results and the manuscript.

Data availability

All data of this study are available from the corresponding author on reasonable request.

Competing interests

The authors declare no competing interests.

Footnotes

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

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Associated Data

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Supplementary Materials

Supplementary material 1 (PDF 289.1 kb) (289.1KB, pdf)

Data Availability Statement

All data of this study are available from the corresponding author on reasonable request.

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