# Corrosion failure analysis of printed circuit boards exposed to H2S resulting from the decomposition of sargassum algae

Benoit Lescop, Olivia Amintas, Carole Boullanger, Stéphane Rioual

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Benoit Lescop, Olivia Amintas, Carole Boullanger, Stéphane Rioual. Corrosion failure analysis of printed circuit boards exposed to H2S resulting from the decomposition of sargassum algae. Microelectronics Reliability, 2025, 170, pp.115784. 10.1016/j.microrel.2025.115784. hal-05061164

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Research Paper

# Corrosion failure analysis of printed circuit boards exposed to H₂S resulting from the decomposition of *sargassum* algae

Benoit Lescop<sup>a,*</sup>, Olivia Amintas<sup>b</sup>, Carole Boullanger<sup>b</sup>, Stéphane Rioual<sup>a</sup>

## ARTICLE INFO

Keywords:

Atmospheric corrosion

Sargassum algae

Microelectronics

H₂S

Corrosion sensors

## ABSTRACT

This work analyzed the corrosion failure of a printed circuit board (PCB) exposed to atmosphere of the island of Martinique (located in the Caribbean Sea). This island suffered from the stranding of *sargassum* algae, which decompose and release toxic gases such as hydrogen sulfide (H₂S). The morphology and properties of the corrosion products were determined using visual inspection, Scanning Electron Microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). Sulfur species were observed in corrosion products, demonstrating the impact of *sargassum* stranding on air corrosivity. RFID silver corrosion sensors were installed to study the corrosion rate in Martinique. X-ray diffraction (XRD) analysis of the sensors confirmed the impact of hydrogen sulfide on corrosion.

## 1. Introduction

A printed circuit board (PCB) is a collective array of electrical circuits assembled on generally a fiberglass-reinforced epoxypolymer panel [1]. PCBs contain various electrical components including resistors, capacitors, transistors and diodes, which are connected to each other by copper traces with tin-based soldered junctions. More than 90 % of PCBs are used in the semi-closed atmosphere environment and are inevitably affected by the negative environmental factors including high humidity rate, condensation, chloride, sulfur pollution ... [2-4]. The corrosion process leads to deterioration of conductive properties of layers and failure of electronic boards. International standards for electrical and electronic related equipment (contact durability) are published by the International Electrotechnical Commission (IEC). The most conventional corrosion tests are continuous salt spray tests (IEC 60068-2-11), alternating immersion of objects in a salt solution followed by drying (IEC 60068-2-52), mixture of gas corrosion test (IEC 60068-2-60), ... [5]. Takano and Mano [6] concluded that failures in electrical contacts and connectors were due to copper corrosion with the consequent formation of copper oxide (Cu₂O). The utilization of machine learning was recently applied to predict PCB failure under corrosive condition [7]. Corrosion leads to a reduction in the lifetime of electronic systems. Tropical environments are particularly prone to corrosion due to high temperatures and humidity rate [8-10].

Martinique is an island located in the center of the Caribbean Sea and has a harsh tropical marine climate due to a high relative humidity (about 75 %) and temperatures constant all year-round 30 °C. These climatic conditions have always been favorable to corrosion. However, for the past 10 years, abnormally premature degradation of electronic devices was reported by people living near Atlantic coast. The situation is accompanied by public health problems [11]. These troubles are consistent with the stranding of tons of *Sargassum* algae on the coasts, which release toxic gases such as hydrogen sulphide (H₂S) or ammonia (NH₃) during their decomposition. Recently, our group studied corrosion process of Cu, Zn and steel by placing coupons on different sites in Martinique during 1 year [12-14]. The unexpected reported corrosion rates in the sites impacted by *Sargassum* stranding were correlated to the presence of H₂S [12-14]. Several studies have already been carried out on the atmospheric corrosion of copper in the presence of H₂S alone under indoor conditions with controlled parameters (concentration, temperature, humidity, etc.) and the corrosive aggressiveness of these gases towards copper has already been demonstrated [15-18]. The reported corrosion products were dominated by covellite (CuS). Moreover, Zou et al. [19] have reported the impact of H₂S on the lifetime of PCB. So, the strong corrosion reported can be linked to the observation of people living near these sites: regular electronic breakdown of electrical devices.

It is of a crucial interest to use sensors to determine the corrosiveness

<footnote><sup>a</sup> Univ Brest, Lab-STICC, CNRS, UMR 6285, F-29200 Brest, France</footnote>

<footnote><sup>b</sup> Madinin'air, 31 Rue Professeur Raymond Garcin, Fort-de-France 97200, France</footnote>

<footnote>* Corresponding author at: LabSTICC, UFR Sciences et Techniques, 6 av. Le Gorgeu, 29200 Brest, France.
E-mail address: benoit.lescop@univ-brest.fr (B. Lescop).</footnote>
of the atmosphere in the vicinity of the PCB and thus control their
lifespan. However, manufacturing mimetic sensors is always a tricky
business. Sensor materials are not always identical to the target material
(PCB copper in this case). The key parameter of the reported high cor-
osivity in Martinique is the high H₂S concentration (few ppm) in the
atmosphere. So, due to its high sensitivity to H₂S, silver is a good
candidate to be integrated into corrosion sensors. Our group developed
corrosion sensors based on RFID (RadioFrequency IDentification) tech-
nology [20]. These sensors were developed to assess air quality and have
been applied in real-life situations to determine corrosion classes in
several museums [21,22]. The principle of the sensors is based on the
electromagnetic coupling between the antenna of the RFID tag and a
metallic sensitive thin film, which acts as a coupon exposed to the
environment. Before exposure, the conductive layer hinders the signal to
reach antenna. During corrosion, metallic layer is transformed to
semiconductor or insulator. So, the RFID tag may respond. Knowing the
initial thickness of metallic coupons, it is possible to obtain metallic
thickness loss. Wireless and low-cost silver sensors were deployed in
different sites in Martinique.

In light of the aforementioned considerations, this study investigates
the effects of the corrosion on a failed PCB used in Martinique. The PCB
is analyzed by visual and microscopic (Scanning Electron Microscopy
and Energy Dispersive X-Ray Spectroscopy) evaluations. Moreover, 30
nm-Ag RFID corrosion sensors are used to confirm the high atmosphere
corrosivity. Sensors were positioned at three different sites in
Martinique and sensors analyzed by XRD (X-Ray Diffraction).

## 2. Experimental details

### 2.1. Exposition

To understand the premature degradation of electronic devices in
Martinique (French west indies), a failure PCB was studied. The board's
function was disturbed after almost 6 years of service in the environment
near Frégate est (presented Fig. 1a). The atmosphere at this site is
considered as tropical (high temperature about 25 °C during all the year
and a high humidity rate) and marine (high chloride ions concentra-
tions) near the seashore, where the *sargassum* algae stranding is re-
ported. The atmosphere is then the tropical atmosphere with the H₂S
pollution. Fig. 1b presents photograph of the board. Typically, several

spots appear at the surface, even visible to the naked eye due to envi-
ronmental corrosion attack.

### 2.2. RFID corrosion sensors

The temperature and relative humidity in Martinique are homoge-
neous and very high (evaluate between 25 °C to 35 °C and 75 %) due its
geographical position. The air corrosivity in three different sites in
Martinique was estimated using RFID corrosion sensors [20]. The sites
shown Fig. 1a are Frégate est, Pointe rouge (west coast impacted by
sargassum stranding) and Fort de France (indoor urban atmosphere).
Fig. 2a shows a photograph of the RFID sensor, it consists of two RFID
tags: a reference tag and a sensitive tag. The chosen reader is a portable
CS 108 model from Convergence Systems Limited connected to a mobile
phone by Bluetooth. The RSSI (Received Signal Strength Indicator) value
and identification number associated with the tags appears on the mo-
bile. The power received from the reference tag was fixed at –43 dBm.

<figure><img src="image_2.png" /><figcaption>Fig. 2. a. RFID corrosion sensor before exposure; b. RFID corrosion sensor at Pointe Rouge during exposure.</figcaption></figure>

<figure><img src="image_3.png" /><figcaption>Fig. 1. a. Map of Martinique, including the positions of the different sites studied, b. Picture of the PCB after exposure.</figcaption></figure>
The chosen sensitive metal is silver due to its high sensitivity to H₂S. The thickness was 30 nm of silver to quickly acquire data. Silver layers were deposited on polycarbonate substrates by DC (Direct Current) magnetron sputtering (PRO line, Lesker). For sputtering deposition, the working chamber was vacuumed to reach a base pressure of 3.10⁻⁷ mbar. During deposition, the substrate rotates at 10 rpm at a distance of ca. 10 cm parallel to the Ag target surface (diameter: 3 in.). Films were deposited in Argon plasma (purity 99.999 %). During deposition, the pressure was kept at 4.10⁻³ mbar. The input power at the target was 75 W.

## 2.3. Characterization of the corrosion products

The morphological and chemical analysis of the corrosion products were carried out, respectively, by scanning electron microscopy (SEM, S800, Hitachi), by energy dispersive X-ray spectroscopy (EDS) and by X-Ray Diffraction (XRD) using PANalytical Empyrean apparatus with CuK radiation (1.5408 Å).

# 3. Results and discussion

## 3.1. Optical analysis of exposed PCB

Fig. 1b shows picture of the PCB. The existence of corrosion products is clearly reported on metal part on the board and different components. To improve understanding of the corrosion process, Fig. 3 presents images from optical microscope. These images confirm the corrosion attack near different components such as C20, R1, R2.

## 3.2. SEM/EDS analysis of exposed PCB

To examine the corrosion process, the corroded surfaces were studied by SEM technique. Fig. 4 presents surface photograph of C20 component (a) and part of metallic zone (b) observed Fig. 1b. The effects of corrosion are clearly seen, in agreement with the reported failure.

To characterize the corrosion products, EDS spectra were acquired on different parts of the PCB. The main reported elements are oxygen and carbon coming from the polymer panel. The conductive layers near the components mainly consist of copper and tin. Additional elements such as sodium, chloride, sulfur can be attributed to corrosion products. The presence of the latter elements is in agreement with the proximity of sea water and the *sargassum* stranding.

Because of the inhomogeneity of the PCB, the determination of the corrosion products can only be realized by EDS mapping. Fig. 5 shows mapping of the C20 component of Cu, Sn, O and S. The localization of tin is well established on the sides of the component to do electric connections. Copper is restricted to several zones near tin always for the connection. Oxygen atoms are mainly localized on the polymer but also on the component. Oxygen atoms seem not interact with tin. The most intense sulfur zones are correlated to the presence of copper and a little

oxygen. This result is accord with the works of Salahinejad et al. [1] and Vogel [23], who reported copper sulfide as major corrosion product in H₂S atmosphere. This can also be consistent with the observations on copper coupons of Becker et al. [17] in H₂S controlled atmosphere and Said Ahmed et al. [12] in real exposition in Martinique. One should note that the presence of copper oxide and/or sulfate is also possible but only in trace form [12]. Moreover, traces of Na and Cl were reported but no localization is well established due to the very weak intensities of these elements.

To confirm the reactivity of copper on H₂S, unprotected copper layers were studied. Indeed, different test points exist in the reverse side of the PCB. They consist of unprotected copper vias. Fig. 6a presents SEM image of test points TP9 and TP10. Fig. 6b-d present mapping corresponding to the most intense elements (excepted carbon). As supposed, one should note the absence of tin. Copper is clearly localized at the connection points. Oxygen elements are seen on the board but also linked to copper, while S is more connected to copper. These observations confirm the existence of CuS and possibly CuSO₂, in line with previously published results for the real case in Martinique [12].

The experiments were repeated on different components like R1, R2 and on the protective steel part seen Fig. 1b. The S presence seems to be correlated with copper rather than tin and the Cu/S ratio is of about 1 in agreement with the possibility of covellite as corrosion products. Concerning the protective steel part, EDS measurements show the existence of Fe, Cr, Ni and elements induced by the corrosion process: Cl and S. The presence of these elements is related to sargassum stranding on the coast. Moreover, this is in agreement with the results of Said Ahmed et al. [14] on steel under real conditions in Martinique. These results confirm the probable impact of H₂S pollution induced by *sargassum* stranding on electronic devices failure.

## 3.3. Use of RFID corrosion sensor in real case

To report the impact of H₂S on corrosion, RFID corrosion sensors were used. The chosen metal is silver due to its high sensitivity to H₂S. Fig. 7 shows pictures after complete corrosion of the sensors. Visually, the corrosion products seem to be dependent to the exposure site.

The initial silver thickness of RFID coupon was 30 nm. During exposure, when the sensitive tag responds, it firstly corresponds to a conductive silver thickness less than 7.5 nm [21]. In this study, the end of the experiment corresponds to a thickness loss of about 22.5 nm. Table 1 presents the duration time between the start of exposure and the responds of the sensitive tag in the three sites. In Frégate est and Pointe rouge, the tag firstly responded after 9 days at the interrogation. The corrosion rate can be estimated to be more than 0.9 µm/year. One should note that both sites present equivalent conditions (short distance to the seawater, temperature ...). In Fort de France, the reaction time was 1 month; so, the thickness loss can be estimated to 265 nm/year. This lower value can be attributed to the higher distance from the sea and so to the *sargassum* stranding.

<figure><img src="image_4.png" /><figcaption>Fig. 3. Optical images of PCB components.</figcaption></figure>
<figure><img src="image_5.png" /><figcaption>Fig. 4. SEM images after exposure of (a) the C20 component and the metallic part (b) of the board.</figcaption></figure>

<figure><img src="image_6.png" /><figcaption>Fig. 5. EDS maps of the C20 component after exposure showing the distribution of Sn (a), Cu (b), O (c) and S (d).</figcaption></figure>

To determine the composition of the corrosion products, EDS analysis of coupons was performed. The presence of Ag, C and O is reported in all the sites, because of the initial silver on polycarbonate layer. Concerning sensors exposed at Fort de France, no additional elements were reported. The corrosion process is so driven by oxidation and the corrosion products should be silver oxide, hydroxide and/or carbonate. This is consistent with the high distance from the seawater. Coupons coming from the other sites present other elements: S, Na, Cl. This proves that near the coasts, corrosion is governed by chloride and sulfur.

Fig. 8 shows diffractograms of coupons exposed at the three sites. All the diffractograms present two broad structures attributed to polycarbonate substrate at about 26° and 42°. At Fort de France, structures attributed to pure silver and oxide are reported. This is in agreement with our EDS data and also with observations of the real atmosphere where silver oxide is reported [24,25]. Data extracted from the Frégate Est and Pointe Rouge sites are close to one another: they present the formation of Ag₂S and the presence of NaCl. One can note that the weak peaks intensity of reported acanthite peaks can be explained by the low thickness of silver metal initially deposed. The presence of salt on the

sensors can be explained by sea spray. The corrosion products are Ag₂S in acanthite phase. The sulfidation process may occur via different pathways but leads always to the formation of Ag₂S on the surface [17]. In the proposed mechanisms [26], sulfur from the dissociation of H₂S may react with metallic ions and the formation of Ag₂S can be described by Eqs. (1) to (3):

$$H_2S \rightarrow H^+ + HS^- \quad (1)$$

$$HS^- \rightarrow H^+ + S^{2-} \quad (2)$$

$$2 Ag^+ + S^{2-} \rightarrow Ag_2S \quad (3)$$

One should note that Ag₂S formation can also be formed by the direct reaction between bisulphide anions (HS⁻) and silver cations (Ag⁺) as reported by Conyers et al. [27].

Our results are coherent with the data reported by Becker et al. [17] in high concentration of H₂S. However, Sanders et al. [28] have reported other corrosion products on silver exposed to various outdoor sites by X-ray Photoelectron Spectroscopy: AgCl, Ag₂SO₄, Ag₂S, AgCO₃ ... They
<figure><img src="image_7.png" /><figcaption>Fig. 6. SEM of the test points TP9, TP10 (a) after exposure and EDS maps showing the distribution of, Cu (b), O (c) and S (d).</figcaption></figure>

<figure><img src="image_8.png" /><figcaption>Fig. 7. Pictures of sensors after exposure in (a) *Fort de France*, (b) *Frégate est* and (c) *Pointe rouge*.</figcaption></figure>

<table><caption>Table 1.</caption><thead><tr><td>Site</td><td>Frégate est</td><td>Pointe rouge</td><td>Fort de France</td></tr></thead><tbody><tr><td>Reaction time</td><td>9 days</td><td>9 days</td><td>1 month</td></tr></tbody></table>

have postulated that silver oxide is a precursor of silver sulfite and/or sulfate. The XRD data presented in Fig. 8 show traces of silver oxide but not silver sulfate. Presumably, the short exposure time (a few days) may not be sufficient to produce observable silver sulfate by XRD [25]. Consequently, our results show that Ag₂S layers are the main corrosion products near the coasts of Martinique, where H₂S concentration is high (over 1 ppm). Deploying RFID Ag-sensor can enable local monitoring of air corrosivity induced by *sargassum* stranding and thus anticipate any

possible failure of electronic cards.

4. Conclusion

The effect of corrosion on a failed PCB used in the Atlantic coast of Martinique was studied using visual and microscopic (SEM and EDS) techniques. These analyses revealed the presence of copper-bound sulfur in the corrosion products. Sulfur-based corrosion products originate from H₂S emission caused by *sargassum* seaweed stranding. To measure the corrosiveness of the air, various RFID corrosion sensor were placed in Martinique. XRD analysis of the sensitive part of the sensors confirmed the presence of sulfur near the coast. PCB protection against corrosion is well known on the coasts of the Caribbean islands: high temperature, high relative humidity, high solar radiation, salinity.
<figure><img src="image_9.png" /><figcaption>Fig. 8. DRX diffractograms of sensors from (a) Fort de France, (b) Frégate est and (c) Pointe rouge.</figcaption></figure>

However, PCB protection needs to be improved to take H₂S gas into account.

### CRediT authorship contribution statement

**Benoît Lescop:** conceptualization; validation; investigation; writing—original draft; writing—review and editing; visualisation; supervision. **Olivia Amintas:** investigation; writing—review and editing. **Carole Boullanger:** investigation; writing—review and editing; supervision. **Stéphane Rioual:** conceptualization; validation; investigation; writing—review and editing; visualisation; supervision.

### Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

### Acknowledgment

The authors would like to thank the Territorial Authority of Martinique (CTM) and the French National Research Agency (ANR) for their financial support through the project N° ANR-19-SARG-0006 (Impact des composes chimiques issus de la décomposition des sargasses et role des microorganismes sur la corrosion des matériaux métalliques. Considérations phénomélogique et juridique – CORSAIR).

### Data availability

Data will be made available on request.

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