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Aging assessment of silicone rubber materials under corona discharge accompanied by humidity and UV radiation

This article has been retracted. Retraction note.
  • Atif Mahmood , Ahmed Muneeb , Usman Saeed , Shahid Alam EMAIL logo , Essam A. Al-Ammar , Jee-Hyun Kang , Wail Al Zoubi EMAIL logo and Dongwhi Choi EMAIL logo
Published/Copyright: August 19, 2024
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 13 Issue 1

Abstract

High voltage (HV) outdoor insulators are subjected to both electrical and environmental stresses, which may lead to their failure. Among the causes, corona discharge, humidity and UV radiation are considered to be the most damaging factors. Efforts are therefore underway to investigate new materials for improving the performance of insulating systems. In this research work, silicone-based room temperature vulcanized samples filled with alumina trihydrate (ATH), silicon dioxide and magnesium hydroxide (MH) were prepared and exposed to AC corona discharge for a duration of 110 h. The electric discharge was also accompanied by UV radiation and two different humidity levels. Following aging of the test samples, diagnosis was conducted to assess their integrity. Measurements based on determining the static contact angle demonstrated the loss of hydrophobicity of all the materials, while hydrophobicity recovery phenomena revealed that ATH-doped materials demonstrated a comparatively higher increase in the contact angle than in samples filled with silicone dioxide (silica) and MH. Scanning electron microscopy analysis revealed deep cracks and block-like structures on their surfaces. Similarly, energy-dispersive X-ray analysis indicated the signs of surface oxidation of the aged samples. However, the data of elemental composition exhibited the loss of filler contents as well as that of carbon from the base matrix. The overall assessment showed that resistance to suppress aging is influenced by both the filler type and its concentration in the investigated composites. The ATH-filled composites exhibited outstanding performance when exposed to the rigors of corona discharge and other environmental stresses. This research contributes to materials science and HV engineering by addressing the development of composites for enhanced insulator performance, with future aspects lying in the utilization of nano-composites for advanced functionality and durability.

Keywords: aging; corona discharge; filler; high humidity; hydrophobicity recovery; SEM; oxidation process

1 Introduction

Outdoor insulators are used in the overhead transmission and distribution lines to mechanically support the line conductors and electrically insulate them from the grounded towers. This necessitates that mechanical strength-to-weight ratio, thermal conductivity and breakdown strength of the insulator should be high apart from the low maintenance cost [1]. These properties of materials can be enhanced using different types of fillers, surface treatments and modification in material properties using different strategies [2,3,4]. Moreover, use of certain fillers and treatment methods improve materials’ thermal properties, hydrophobicity and friction coefficient [5,6]. Rubber polymers are employed as insulating materials in high voltage (HV) transmission, the recycling of which are of major importance [7]. Silicone rubber (SIR) is used as an insulator, and these rubber materials have created new opportunities for operating at higher voltages due to their superior hydrophobicity, increased mechanical strength, less maintenance needs and high dielectric strength [8]. Hydrophobicity of SIR is a key characteristic that sets it apart from ceramic and glass insulators and contributes to its better pollution flashover performance [9]. Moreover, its ability to recover hydrophobicity, which is considered as one of the most important characteristics, gives it preference over other polymers. The reason behind it is the migration of pre-existing low molecular weight (LMW) polydimethylsiloxane (PDMS) from the bulk of the material to the degraded surface. This transfer (of LMW) can take place even if the insulator surface is polluted, and due to this advantage, SIR-based insulators are used in highly contaminated areas as well. Moreover, the hydrophobic nature of SIR prevents the development of leakage current, which subsequently inhibits surface flashover [10,11,12]. SIR is a solid insulating material, but there are liquids as well as gaseous materials that provide better insulating properties [13,14].

SIR insulators due to their organic structure are prone to aging and degradation when exposed to electrical and environmental stresses [15,16,17]. A strong electrical field may cause dry-band arcing (DBA) and corona discharge. The loss of hydrophobicity enhances the flow of leakage current which leads to DBA, and eventually to the eroding of insulator’s surface [18]. Similarly, corona discharge due to a locally enhanced electric field is considered as another potential threat to the performance of SIR insulators. The gaseous (NO and NO2) byproducts of corona discharge may combine with the moisture contents to form HNO3, which may be damaging to both the core and the shed material. Moreover, corona discharge also produces ozone gas as well as if it takes place in the vicinity of an insulator it may deposit electrons/ions on its surface [19,20]. The latter has been found to affect the electric field distribution and flashover performance of the insulator [21]. The inescapable and gradual process of aging is inevitably triggered by prolonged and continuous exposure to elevated levels of electric field intensity, high UV radiation, increased humidity, substantial pollution and the presence of various external environmental factors [22,23,24].

Significant work has been done to study the impact of fillers on the performance enhancement of insulating materials under the impact of corona exposure. In the study of Nazir et al. [25], the effectiveness of SIR materials filled with various concentrations of micro-/nanosized silica was assessed in order to determine the most suitable formulation to prevent both the corona discharge and loss of hydrophobicity. Results of the measurements showed that the test sample filled with 5 wt% nano-silica has the higher resistance to corona discharge than the others without any filler as well as those filled with micro- and micro-/nanosilica. Silica fillers not only provide better insulating behavior but also are used to improve resistance against different types of radiation [26]. Nazir et al. used micro-alumina trihydrate (ATH) and nano-alumina for enhancing the properties of SIR against corona discharge. The conducted analysis indicated that addition of a small amount of nano-alumina to the micro-ATH-filled sample significantly improved its performance [27]. In one study, authors used micro-/nanosized silica fillers, and they found that the ability to suppress corona discharge was found to be more for the co-filled composite containing 2 wt% nano-silica and 10 wt% micro-silica as compared to the other formulations [28]. Similarly, hydrophobicity loss and recovery phenomena were studied on SIR samples filled with aluminum hydroxide and fumed silica after being exposed to corona discharge. The authors found that loss of hydrophobicity on a clean surface was more than that on the contaminated surface. Moreover, the hydrophobicity recovery of clean and contaminated surfaces after being exposed to corona was fast returning to the initial value of contact angle just after 24 h of recovery time [29]. In a more recent work, authors studied the impact of humidity, heat and corona discharges on the surface of ATH-filled insulators. They found that due to the synergistic effect of aging the morphology of composites was distorted, precipitation of fillers also occurred and deeper surface cracks were noticed. Infrared spectroscopy shows continuous breakdown of polymer chains. Micro-cavities result from SiR and ATH decomposition, reducing hydrophobicity, increasing moisture absorption, and causing abnormal heating [30].

The efforts made by various researchers have demonstrated, for instance, that corona discharge when combined with the environmental stresses (humidity, acid fog, or vertical wind) have synergistic effects in speeding up the breakdown of insulators [31,32,33]. However, the reported data are not ample, particularly the severity of degradation due to corona discharge under UV radiation and relatively high humidity is not studied at length. Accounting for this gap, long term (110 h) AC corona discharge aging of SIR materials reinforced with different concentrations of micro-sized ATH, silica and magnesium hydroxide (MH) fillers was conducted in a specially designed chamber. The experimental setup was also equipped with arrangements for UV radiation and humidity. For the latter, two levels (medium and relatively high) were considered. After performing the aging, test samples were assessed for various properties to describe the insulation characteristics, with particular emphasis on understanding hydrophobicity recovery phenomena using contact angle measurement. The other diagnostic tools employed included scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) spectrometry to analyze the surface morphology and elemental composition, respectively. The results of various tests were demonstrated, discussed and compared to identify the most suitable composition among the investigated formulations to retard the process of aging due to the synergetic impact of electrical and environmental stresses.

2 Materials and tests

2.1 Composite preparation

RTV-615A (RTV = room temperature vulcanized) with a density of 1.15 g/m3 was used as the base material. It contained 70% of PDMS and 30% of vinyl compound. Three types of fillers, silica, ATH and MH, were used for reinforcement of the base polymer. The different tools/equipment used in preparation process of test samples are shown in Figure 1, and the procedure is described as follows. In the first step, filler particles were stirred for 15 min in a 100 ml solution of ethanol, followed by ultrasonication for 30 min to achieve proper de-agglomeration. Then, RTV-615A was added to the filler, and blending was performed using an HSM-100 LSK high-shear blender for 15 min. Following that step, the curing agent (RTV-615B) was added to the mixture, and it was stirred again for 15 more minutes. The part-A to part-B ratio was kept at 10:1. Moreover, to remove any entrapped air, the prepared mixture was placed in a vacuum desiccator for 10 min. Following that, molding was done to get the required shape and size of the test sample. The shape was flat, while dimensions selected were of two types. One was 75 mm × 40 mm × 3 mm and the other was 120 mm × 50 mm × 5 mm. Finally, to complete the vulcanization process, a pressure of 30 MPa was applied using a hydraulic press for 30 min, and then postcuring was performed in an oven at a temperature of 85°C for the next 4 h. The list of prepared room temperature vulcanized silicone rubber (RTV-SiR) composites is given in Table 1.

Figure 1 (a) Schematic view and (b) photographic representation of the corona discharge setup. Needle-plane electrodes for aging the test samples are shown. Also, arrangements for UV irradiation and humidity are shown.
Figure 1

(a) Schematic view and (b) photographic representation of the corona discharge setup. Needle-plane electrodes for aging the test samples are shown. Also, arrangements for UV irradiation and humidity are shown.

Table 1

Specifications of the studied SIR materials reinforced with different concentrations of ATH, silica and MH fillers

Sample notation RTV-SIR (wt%) Filler specifications
Type Particle size (µm) Specific gravity (g/cm3) wt%
A50 50 ATH 1.7 2.40 50
S50 50 Silica 1.1 2.65 50
M50 50 MH 1.1 2.40 50
A40 60 ATH 1.7 2.40 40
S40 60 Silica 1.1 2.65 40
M40 60 MH 1.1 2.40 40

2.2 Corona discharge setup

Specifications of the studied RTV-SIR materials reinforced with different concentrations of micro-sized particles of silica, ATH and MH are provided in Table 1. Samples of materials were prepared in a rectangular shape having a length, width and thickness of 120 mm, 50 mm and 5 mm, respectively, and exposed to AC corona discharge using a needle-plane electrode arrangement, as shown in Figure 1. The whole setup was housed in a stainless-steel chamber, where a regulated gaseous environment was provided to minimize possible ozone impact on the conducted measurements. The needle electrode with a tip diameter of 2 mm served as a corona source. The test sample was placed on the bottom electrode, which was grounded. The schematic and pictorial views of the corona discharge setup are shown in Figure 1, and the procedure for corona discharge is described as follows. Six single needle-plane identical electrodes connected to a 16 kVA transformer were used to expose the test samples to corona discharge. The applied voltage was adjusted with the help of a variac (regulating transformer).

The voltage value was measured through a HV probe, which was further connected to an oscilloscope for displaying the data. The scale-down ratio of the probe was 1,000:1. Corona discharge was created at two different electric field strengths by adjusting the gap distance between the tip of the needle electrode and the sample’s surface as 1 and 5 mm. Moreover, to incorporate the effect of UV radiation, UVA-340 lamps were used. However, for controlling the humidity level, a humidifier equipped with a sensor, display and controller was placed inside the chamber. Experiments were performed at two different relative humidity levels, medium (55–65%) and high (75–85%). Also, to check the variation of results, measurements were repeated at least three times.

2.3 Hydrophobicity loss and recovery analysis

It is crucial to assess the hydrophobicity of insulating materials as it reduces with the aging process. Numerous techniques, including the water immersion technique; sliding angle, dynamic contact angle, and static contact angle measurement; and the Swedish Transmission Research Institute scale can be used to quantitatively evaluate the hydrophobicity loss and recovery. Among these, the most popular method is the measurement of static contact angle, which is present at the point where a liquid drop meets a material surface. The following Young–Dupré equation is used to link the contact angle with the surface energy of the solid and surface tension of the liquid materials:

γ GS = γ SL + γ LG cos θ ,

where γ GS , γ SL and γ LG represent the interfacial tensions in-between gas and solid, solid and liquid and liquid and gas, respectively, and θ denotes the contact angle.

Due to the high surface energy and ease of wetting, hydrophilic materials allow water droplets to touch more surface area, and the contact angle ultimately decreases from 90°. Hydrophobic materials, on the other hand, have low surface energies that prevent water droplets from flowing along their surfaces, causing the contact angle to be greater than 90° [34].

In the present study, a micropipette was used to put a drop of 20 µl size to measure the contact angle of SIR materials. Following corona aging of the test sample, a droplet of de-ionized water was placed on its surface, and a snapshot was captured through a high-resolution camera, which was further uploaded to a computer. “ImageJ” software having low-bond axisymmetric drop shape analysis plugin was used to find the static contact angle of the droplet [35]. Moreover, to assess hydrophobicity recovery of the aged samples, measurements were taken at different time intervals. The recorded data were also compared with that of the unaged (virgin) materials.

2.4 SEM and EDX analyses

SEM is a diagnostic technique used for assessing surface topography in order to evaluate the morphology of materials under study. Moreover, it is also used to identify any changes on the surface of the treated/aged sample. In the test procedure, to create SEM micrographs, a high-energy beam of electrons scans the sample in a raster scanning pattern. In order to produce signals that contain information about the sample’s surface topography and composition, the beam of electrons interact with the atoms of samples on the surface. In the present study, an FEI Quanta FEG-250 ESEM machine, which was also equipped with an EDX detector, was used to generate high-quality SEM micrographs to assess the morphology of the sample as well as to measure the compositions of elements on its surface. For comparative analysis, SEM images were taken both for the unaged and corona aged SIR materials.

3 Results of diagnostic measurements

3.1 Loss of hydrophobicity

Contact angles were measured both prior to and postcorona discharge aging of the test samples. The collected data under different studied scenarios are shown in Tables 2 and 3. As seen in both the tables, the contact angle of untreated (unaged) samples is greater than 90°, showing their good hydrophobicity. However, due to the long time (110 h) exposure of test samples to corona discharge and other stresses (humidity and UV radiation), their hydrophobicity reduces (contact angles are lower than those of the unaged materials). This observation is the same, irrespective of the reinforcement of samples with the type and concentration of fillers. Nevertheless, the decrease in contact angle due to aging is different for the SIR materials, which is dependent on their composition. It is lower for ATH-doped samples A50 and A40 as compared to their silica and MH-filled counterparts, respectively, reflecting better hydrophobicity of the former than the latter. The performed measurements also indicate the effects of UV radiation, humidity and electric field stress (different at 1 and 5 mm gap distances). For example, the loss under high humidity is more than that under medium humidity. Moreover, by adding UV radiation, the impact becomes stronger. As far as the effect of varying gap distance is concerned, higher loss can be noticed at 1 mm as compared to that at 5 mm.

Table 2

Measured contact angle of the test samples before and immediately after their corona aging

Samples Unaged High humidity (with UV) High humidity (without UV) Medium humidity (with UV) Medium humidity (without UV)
A50 95.6° 20.2° 21.7° 21.6° 22.4°
S50 93.8° 13.7° 14.9° 20.8° 23.4°
M50 95.3° 15.8° 16.4° 16.1° 22.8°

Data recorded at medium and relatively high humidity levels as well as with and without UV radiations are shown.

Table 3

Measured contact angle of the studied SIR materials before and immediately after their corona aging at 1 mm and 5 mm gap distances between the needle electrode and sample’s surface

Samples Unaged 5 mm (with UV) 5 mm (without UV) 1 mm (with UV) 1 mm (without UV)
A40 92.1° 32.8° 35.9° 26.3° 27.9°
S40 97.0° 24.4° 30.2° 23.3° 23.7°
M40 99.5° 22.9° 28.6° 22.1° 23.1°

3.2 Hydrophobicity recovery

Hydrophobicity recovery is one of the desired properties of SIR insulators, and to analyze the factors behind it, an in-depth study was performed in the current research. For this purpose, contact angles of the unaged and corona aged SIR materials were measured using the procedure described in Section 2.2. Collected data of the test samples exposed to corona discharge under relatively high humidity (75–85%) and UV radiation containing 50 and 40 wt% concentrations of the studied fillers are shown in Figure 2(a) and (b), respectively. As is seen, contact angles of the test samples recorded through the first (immediately after aging) and the last measurements (at 100 h) are different. The latter values are higher than the earlier ones, reflecting the hydrophobicity recovery phenomenon. Moreover, analyzing the recovery rate through slopes of the lines, one can observe that, in general, it is higher for SIR materials reinforced with 40 wt% of fillers as compared to their 50 wt% doped counterparts, particularly at the beginning. Similarly, for samples S40 and M40, the final mean values (of angles) of 72.3° and 70.7°, respectively, are also more than those of S50 and M50, which are 69.7° and 65.6°, respectively. The only exception is that of A40 and A50, where for the latter an angle of 75.7° was recorded, while for the earlier, it was measured as 74.5°. To analyze the impact of varying humidity levels (during corona discharge under UV radiation) on the hydrophobicity recovery rate, the contact angle vs recovery time graph of sample A50 (filled with 50 wt% of micro-sized ATH) is shown in Figure 3. As is seen, both the initial and final values as well as slopes of the curves in various time intervals are different under medium (55–65%) and relatively high humidity (75–85%) levels. For instance, in the beginning, the recovery rate shown by the black and red lines is quite similar, although mean values of angles are higher under medium humidity as compared to the high humidity. On the other hand, later on, opposite tendency/behavior is noticeable. Both the slope of the curve and contact angle become higher under the humidity level of 75–85% than that of 55–65%. The presented data thus infer that hydrophobicity loss increases when corona discharge is accompanied by high humidity (as is also summarized in Table 2); however, under the same conditions, the recovery phenomenon after certain time duration is also the fastest.

Figure 2 Hydrophobicity recovery of the corona aged SIR materials under high relative humidity (75–85%) and UV radiation. Sub-figures (a) and (b) show measurements for the samples containing 50 and 40 wt% concentrations of the studied fillers, respectively.
Figure 2

Hydrophobicity recovery of the corona aged SIR materials under high relative humidity (75–85%) and UV radiation. Sub-figures (a) and (b) show measurements for the samples containing 50 and 40 wt% concentrations of the studied fillers, respectively.

Figure 3 Hydrophobicity recovery of the test sample A50 exposed to corona discharge under UV radiation at 1 mm gap distance and at two different humidity levels.
Figure 3

Hydrophobicity recovery of the test sample A50 exposed to corona discharge under UV radiation at 1 mm gap distance and at two different humidity levels.

In addition to the varying humidity level, the effect imposed by the UV radiation together with the corona discharge was also assessed on the studied SIR materials. One such example is shown in Figure 4, where data for the ATH-doped test sample A40 are presented. For comparative analysis, measurements taken without applying any UV radiation are also displayed. As is seen, there is a clear difference between the two curves and remains almost consistent throughout the length of the data recording time, indicating that both the hydrophobicity loss and its recovery rate are adversely affected when corona discharge is accompanied by UV radiation.

Figure 4 Hydrophobicity recovery of the SIR material A40 aged under high humidity at 1 mm gap distance. Data recorded both with and without UV radiation are displayed.
Figure 4

Hydrophobicity recovery of the SIR material A40 aged under high humidity at 1 mm gap distance. Data recorded both with and without UV radiation are displayed.

To examine how the strength of the electric field stress influences the contact angle as well as its increase (recovery) after corona discharge, data were recorded at 1 and 5 mm gap distances between the needle tip and the sample’s surface. For illustration, measurements performed on SIR material M40 reinforced with 40 wt% of micro-sized MH filler are shown in Figure 5. It is worth highlighting here that corona discharge aging was realized under UV radiation and high humidity to create the worst impact. As is seen, by increasing the electric field stress through reducing the gap distance, the effect becomes stronger. Thus, contact angles throughout the duration of measurement are high (showing high hydrophobicity) when the sample is stressed at 5 mm as compared to 1 mm. However, the slopes of the curves, representing the hydrophobicity recovery rate, are nearly the same.

Figure 5 Hydrophobicity recovery of SIR material M40 aged under UV radiation and high humidity. Data recorded at 1 and 5 mm gap distances between the sample and the needle electrode are shown.
Figure 5

Hydrophobicity recovery of SIR material M40 aged under UV radiation and high humidity. Data recorded at 1 and 5 mm gap distances between the sample and the needle electrode are shown.

In Figure 6, two curves of the test sample doped separately with 40 and 50 wt% concentrations of the MH filler are shown. Corona discharge treatment was done at 1 mm gap distance and under UV radiation and high humidity to see how the severity of this worst condition is reduced by varying the filler concentration. By analyzing the curves, it can be inferred that apart from the high contact angles in the entire time window, the recovery rate is also fast for the sample M40 compared to that of SiR M50, particularly, at the beginning. Thus, reinforcement of the base material with the optimal concentration of filler is important for achieving desired results. Moreover, it is concluded from the analysis of data in this section that corona discharge treatment of the test samples accompanied by environmental and electrical stresses adversely affect their hydrophobicity as the contact angle did not reach 90° in any of the studied scenario in the whole recorded time.

Figure 6 Hydrophobicity recovery of corona exposed SIR materials M40 and M50. Aging is performed under high humidity and UV radiation and at 1 mm gap distance.
Figure 6

Hydrophobicity recovery of corona exposed SIR materials M40 and M50. Aging is performed under high humidity and UV radiation and at 1 mm gap distance.

3.3 SEM analysis

SEM micrographs of the corona aged SIR materials were obtained using the procedure outlined in Section 2.3. The collected data were analyzed under different studied scenarios to assess/compare the effects of various stresses/environmental factors (electric field, UV radiation and humidity) on the severity of surface degradation. SEM images of unaged samples are presented in Figure 7. However, Figure 8 depicts the surface morphology of ATH, silica and MH-doped samples A50, S50 and M50, respectively, which were aged under an HV electrode through corona discharge at 1 mm gap distance. Effects of UV radiation as well as those of the medium and high humidity levels were also incorporated. As is seen, the synergetic impact of these stresses affects the surface conditions, even though the severity is different being dependent on the material’s composition. For the test sample A50, surface cracks and fissures can be observed which become deeper when the humidity level is increased (compare images in Figure 8(a) and (b)). A similar tendency is also indicated in Figure 9(d) and (e), where the results of SIR material M50 are displayed. Nevertheless, surface degradation/roughness of the ATH-filled sample is less pronounced as compared to its MH-filled counterpart. The relatively strongest effect is demonstrated in Figure 8(e) for material M50. For the silica-doped material S50, its SEM micrograph is provided in Figure 8(c), in which signs of surface deterioration are also noticeable, though they are much weaker than those in Figure 8(e).

Figure 7 SEM micrographs of unaged composites: (a) A40, (b) S40, (c) M40, (d) A50, (e) S50 and (f) M50.
Figure 7

SEM micrographs of unaged composites: (a) A40, (b) S40, (c) M40, (d) A50, (e) S50 and (f) M50.

Figure 8 SEM micrographs of the studied composites aged under corona discharge at 1 mm gap distance and under UV radiation. Sub-figures (a) and (b) represent data of sample A50 under high and medium humidity levels, respectively, (c) displays the image of sample S50 under high humidity and (d) and (e) show images of sample M50.
Figure 8

SEM micrographs of the studied composites aged under corona discharge at 1 mm gap distance and under UV radiation. Sub-figures (a) and (b) represent data of sample A50 under high and medium humidity levels, respectively, (c) displays the image of sample S50 under high humidity and (d) and (e) show images of sample M50.

Figure 9 (a) Image of the corona aged SiR material M40 at 5 mm gap distance and under UV radiation. (b) and (c) SEM micrographs of the test sample M40 at 1 mm gap distance and without and with UV radiation, respectively. (d) and (e) Data of samples S40 and A40 at 1 mm gap distance and under UV radiation. The humidity level in all these scenarios was kept high (75–85%).
Figure 9

(a) Image of the corona aged SiR material M40 at 5 mm gap distance and under UV radiation. (b) and (c) SEM micrographs of the test sample M40 at 1 mm gap distance and without and with UV radiation, respectively. (d) and (e) Data of samples S40 and A40 at 1 mm gap distance and under UV radiation. The humidity level in all these scenarios was kept high (75–85%).

To examine the impact of electric field strength, which was varied through changing the gap distance, on the surface degradation, SEM images of SIR materials reinforced with 40 wt% concentration of the studied fillers are presented in Figure 9. Effects with and without UV radiation and by keeping high humidity level were also assessed. A comparison of the sub-figures shows that by applying the extreme/worst conditions (UV radiation and adjusting the gap distance at 1 mm which gives a strong electric field), more surface roughness in the form of deep cracks, block-like structures and even spots of white powder are created, resulting in the highest loss of hydrophobicity.

This is illustrated in Figure 9(c) for the ATH-doped material A40. However, the data (of the same sample and at the same electric field) recorded without UV radiation show comparatively much lower surface degradation, as is evident from Figure 9(b). On the other hand, if the electric field is reduced (by increasing the gap distance to 5 mm) while keeping UV radiation, no significant change occurs. This can be observed from the comparison of images in Figure 9(a) and (c). For other studied materials S40 and M40, SEM micrographs are provided in Figure 9(d) and (e), respectively, which also exhibit signs of surface roughness (shallow cracks and even white spots), although weaker as compared to sample A40. It is thus concluded from the analysis of data in this section that corona discharge when accompanied by UV radiation imposes a stronger impact than other stresses/environmental factors (electric field and humidity).

3.4 EDX analysis

To identify changes in the elemental composition of the investigated materials, EDX analysis was performed both prior to and post corona aging tests. Results of the measurements are presented in Table 4, where percentage values (of the constituents) of the samples reinforced with 50 wt% concentration of ATH, silica and MH fillers are listed. It is important to highlight here that the major elements constituting the studied composites are silicone (Si), oxygen (O), carbon (C), aluminum (Al) and magnesium (Mg). As is seen, corona discharge treatment affects constituents of the samples including both the fillers and other components, and its intensity increases by combining other stresses/factors with it. For example, the SIR material A50 shows a decrease of both Al (ATH filler) and C. In the case of Al (ATH filler) the percentage drops from 16.38 to 11.69 when effects of UV radiation and high humidity are also incorporated. The percentage of other elements (O and Si), however, increases beyond the level measured in the unaged conditions of the sample. Similarly, by analyzing the data of SIR S50 (containing silica as a filler), similar tendency can be observed, particularly related to the percentage drop of C. The quantity of Si is also reducing, although weakly as compared to C. As far as the MH-filled sample M50 is concerned, the percentage decrease of Mg (filler) is much higher than those of silica and ATH.

Table 4

Elemental composition of the studied SIR materials aged under corona discharge at 1 mm distance between the needle tip and the sample surface

A50 % C % O % Al % Si
Unaged 20.91 38.96 16.38 23.74
Without UV, high humidity 18.35 43.15 14.30 24.20
With UV, high humidity 16.16 47.59 11.69 24.56
Without UV, medium humidity 18.05 43.11 14.78 24.06
With UV, medium humidity 16.20 47.22 11.83 24.75
S50 % C % O % Si
Unaged 24.67 31.99 43.34
Without UV, high humidity 12.25 45.26 42.49
With UV, high humidity 8.26 54.30 39.44
Without UV, medium humidity 11.63 46.16 42.21
With UV, medium humidity 8.73 53.30 37.97
M50 % C % O % Mg % Si
Unaged 23.65 32.32 17.16 26.87
Without UV, high humidity 22.98 37.96 11.62 27.44
With UV, high humidity 17.52 43.77 8.79 29.92
Without UV, medium humidity 23.11 36.21 13.19 27.49
With UV, medium humidity 17.67 43.50 9.19 29.64

Moreover, the loss of carbon content was higher in the case of UV and high humidity. However, O and Si like material A50 show their increase.

To analyze the effect of changing the gap distance in corona discharge tests on the elemental composition of the studied materials, measurements are shown in Table 5. Data were collected while keeping humidity at a relatively high level (75 to 85%). As is seen, varying the electric field strength does create an impact. For example, by reducing the gap distance (giving a higher field), samples lose both fillers and carbon, irrespective of their composition. Moreover, upon worsening the conditions (applying UV radiation and a strong electric field), the percentage of constituents (fillers and carbon) drop further. On the other hand, in assessing the effect on O and Si, similar results as presented in Table 4 can be seen. Thus, their percentage increase by increasing the severity of the synergetic impact of electrical and environmental stresses.

Table 5

Elemental composition of the corona aged test samples under high humidity (75 to 85%)

A40 % C % O % Al % Si
Unaged 23.20 32.92 13.28 30.60
5 mm, without UV 22.56 33.25 12.22 31.97
5 mm, with UV 19.97 37.06 10.17 32.80
1 mm, without UV 17.15 38.77 10.38 33.70
1 mm, with UV 18.47 40.25 9.42 34.86
S40 % C % O % Si
Unaged 26.56 39.61 33.83
5 mm, without UV 24.22 43.31 32.47
5 mm, with UV 20.42 47.27 32.31
1 mm, without UV 23.59 46.87 29.54
1 mm, with UV 19.75 51.27 28.98
M40 % C % O % Mg % Si
Unaged 22.10 31.36 15.84 30.70
5 mm, without UV 18.24 35.34 13.57 31.85
5 mm, with UV 16.61 38.83 12.22 32.34
1 mm, without UV 15.46 39.48 11.41 33.65
1 mm, with UV 14.92 40.71 9.39 34.98

3.5 Discussion

To elaborate/identify possible reasons associated with the important/noticeable findings of various diagnostic measurements, the following discussion is presented. Analysis of the contact angle through which hydrophobicity was determined showed that (immediately after corona discharge aging) ATH-doped samples (A40 and A50) have higher values than their silica and MH-filled counterparts. Moreover, it was found to be affected by the UV radiation, humidity and electric field strength. As far as hydrophobicity recovery (increase in the contact angle with time) is concerned, it was observed to be higher in the initial duration of diagnosis and lower later on, irrespective of the composition of samples. Materials reinforced with a relatively high concentration (50 wt%) of the studied fillers showed comparatively slow recovery. This may be linked with the agglomeration phenomenon, which suppresses the movement/diffusion of LMW from the bulk of material toward its surface. Transfer of LMW, if takes place effectively, enhances the ability of materials to recover their surface characteristics/properties (including hydrophobicity) after being exposed to aging though applying various stresses. Apart from this (movement of LWM), hydrophobicity recovery phenomenon is also attributed to the polar group reorientation and condensation of silanol groups [18]. Quantifying the impact of individual stresses on hydrophobicity recovery, UV radiation was identified as the major (most damaging) factor. Nevertheless, the effect of increasing electric field strength (reducing gap distance) and humidity level was also noticed.

Assessment of the elemental composition of the test samples showed an increase in the oxygen content due to the oxidation process on their surfaces. This increase causes the formation of a hydrophilic layer that resembles silica and polar silanol groups on the PDMS (base matrix in the studied materials) surface, resulting in the loss of its hydrophobicity. The latter was observed to be higher when corona discharge treatment was intensified by adjusting the lower gap distance (between the needle tip and sample’s surface) as well as by applying UV radiation and high humidity. The reason behind the synergetic impact of these stresses, according to the mechanism outlined in the study of Hillborg and Gedde [36], is the strong oxidation process, which causes the transformation of the hydrophobic –CH3 group to the –CH2 group. Moreover, it produces hydroxyl (Si–CH2OH) and peroxides (Si–CH2OOH) due to the reaction between oxygen contents and PDMS. Apart from O, an increase in the silicone contents on the surface of materials was also noticed, which can be attributed to the movement of LMWs. However, for samples S40 and S50 (filler was silica, which comprised both silicone and oxygen), no significant change was recorded, and its interpretation is rather complex due to the difficulty in distinguishing between the movement of LMWs and lowering of the filler content. Opposite to the behavior of O and Si, decreasing percentage of both C and filler was observed, representing a loss of the other desired properties such as electrical and mechanical properties [37].

SEM micrographs, depending on the severity of aging, exhibited deep cracks, pits, block-like structures and even spots of white powder. The development of surface cracks may provide a low resisting route/path to the diffusion of LMW constituents, thus contributing to the higher rate of increasing contact angle (fast hydrophobicity recovery). To increase the recovery rate through cracking the hydrophilic layer on the surface, formed due to aging, Hillborg and Gedde suggested a modest mechanical stress [38]. It was also hypothesized in another research work that corona-induced deformation of the PDMS surface starts the angle recovery process at a faster rate [39].

4 Conclusions

This study focuses on improving certain properties of insulator composites utilizing the concept of materials sciences and providing better materials for HV insulation systems. The effect of the corona discharge accompanied by UV radiation and two humidity levels (medium and high) was analyzed on six different types of SIR materials filled with micro-sized particles of ATH, silica and MH. The duration of the test sample’s treatment was kept as 110 h. Following aging, different tools were employed for diagnosis, particularly to examine hydrophobicity recovery phenomena. The results of performed measurements, carried out immediately after the aging process of samples, exhibited a noticeable decrease of their contact angle. Moreover, the recovery of hydrophobicity on ATH-doped materials was observed at a relatively higher rate as compared to the silica and MH-filled samples. SEM micrographs and other assessments demonstrated the strongest impact of UV radiation among the investigated stresses/factors. Similarly, analysis of the elemental composition revealed the loss/gain of major constituents of the test samples, affecting adversely both their surface characteristics and other desired properties. The overall assessment showed that selection of the optimal weight percentage ratio of the base matrix and filler particles is important for achieving desired results. This research provides foundational insights into improving the insulator composite performance utilizing filler contents with higher concentrations. Future studies could explore hybrid composites having both micro and small concentrations of nano-sized particles to increase the lifespan of insulation systems. Investigating the synergistic impacts of micro- and nano-fillers under multiple stress conditions could completely transform the fabrication technique of futuristic insulating materials for HV insulation systems.

Acknowledgments

The authors are thankful to the Higher Education Commission (HEC), Pakistan, for providing the funds for one year research work. The authors are also thankful to Professor Ayman El-Hag and the University of Waterloo, Canada, for providing the equipment required for this research work and also work space in the high voltage laboratory. This work was supported by Researchers Supporting Project number (RSP2024R492), King Saud University, Riyadh, Saudi Arabia. This work was supported by the National Research Foundation of Korea (NRF) grant funded by the Korea government (MSIT) (No. 2022R1C1C1008831).

  1. Funding information: This work was supported by the Higher Education Commission and GIK Institute under the grant number 119FEG2004. This work was supported by Researchers Supporting Project number (RSP2024R492), King Saud University, Riyadh, Saudi Arabia.

  2. Author contributions: Atif Mahmood: writing – original draft preparation, conceptualization. Ahmed Muneeb: methodology, supervision. Usman Saeed: software, visualization. Shahid Alam: validation, formal analysis. Essam A. Al-Ammar: investigation, data curation. Jee-Hyun Kang: resources, data curation. Wail Al Zoubi: writing – review and editing, funding acquisition. Dongwhi Choi: supervision, project administration. All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2024-01-12
Revised: 2024-03-24
Accepted: 2024-03-25
Published Online: 2024-08-19

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ntrev-2024-0018
Keywords for this article
aging; corona discharge; filler; high humidity; hydrophobicity recovery; SEM; oxidation process
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