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Preparation of hydrophobic silicone rubber composite insulators and the research of anti-aging performance

  • Zhaohua Zhang EMAIL logo
Published/Copyright: November 19, 2024
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e-Polymers
From the journal e-Polymers Volume 24 Issue 1

Abstract

Series of Si75/nZ/tZ@SRHTV materials are prepared by dip-coating method to improve the hydrophobicity and breakage-resistant ability of high-temperature vulcanization silicone rubber (SRHTV) using ZnO particles as UV absorbent and bis(triethoxysilylpropyl) disulfide (Si75) as consolidant. The introduction of tetrapod ZnO can build a bramble structure and endow the SRHTV materials with excellent hydrophobicity. The combined utilization of nano-ZnO and tetrapod-ZnO can endow the SRHTV material well with anti-UV ability, while using Si75 gives the SRHTV materials favorable thermal reparability due to its reconfigurable disulfide bond. The optimal parameters are 10%-Si75, 1%-nZnO, and 50%-tZnO. After longtime UV radiation, this material still shows good hydrophobicity and intact surface. The FTIR and X-Ray diffraction analysis indicate the breakage of Si–O molecular chains and the exposure of inorganic fillers for SRHTV. Compared with the neat SRHTV, the mechanical property of the Si75/nZ/tZ@SRHTV material has no significant change. The research indicates the excellent comprehensive performance of Si75/nZ/tZ@SRHTV materials.

Graphical abstract

Si75/nZ/tZ@SRHTV materials prepared by the dip-coating method using SRRTV as a bonding layer show a rough bramble mastoid structure. Benefiting from the special functional layer structure, this material presents an excellent hydrophobicity, anti-UV aging ability, and thermal reparability.

Keywords: silicone rubber; hydrophobicity; anti-UV ability; thermal-reparability; dip-coating method

1 Introduction

Silicone rubber (SR) is a type of polymer material with high performance (1,2). According to the preparation process, the SR can be divided into high-temperature vulcanization silicone rubber (SRHTV) and room temperature vulcanization silicone rubber (SRRTV) mainly. Both of them have the similar molecular chain structures and chemical characteristics. Generally, the main chain of SR molecular is Si–O bonds with dimethyl or methyl vinyl side chain. To satisfy the needs of the application in insulated power transmission, the methyl vinyl silane is usually used as the raw rubber, and inorganic particles such as Al2O3, Al(OH)3, SiO2, and TiO2 are added as functional fillers to improve its performance, including reinforcement function, anti-UV function, and antioxidation (3,4,5). The SRHTV materials prepared by vulcanization reaction at high temperature and high pressure present excellent performance, such as high-temperature resistance, low-temperature resistance, corrosion resistance, light radiation resistance, mucedine resistance, and pollution flash resistance.

However, limited by its own quality of raw materials and the vulcanization technology, the performance of SRHTV materials is likely to decline sometimes. Besides, the SRHTV applied in the insulation system is usually used outdoors. The aging phenomena including the deterioration of hydrophobicity and the cracking of surface easily occur on the surface of SRHTV materials due to the longtime outdoor applications under solar radiation, rain infiltration, and even air pollution, and thus led to the decreased performance (6,7,8). Even, the skin layer of SRHTV is easily damaged by bird-peck and scratch. In either case, it will accelerate the aging process and cause the severe security incident, which threatens the security of power grid equipment.

Promoting the hydrophobicity or reducing the occurrence of microcracks or repairing the formed cracks by adjusting the surface structure are effective means to improve the performance of SRHTV (9,10). For hydrophobicity improvement, many reported articles focused on the modification of SRHTV surface by the introduction of hydrophobic substance or by the increase of roughness (11,12). The common methods include the surface fluorination and surface etching. For example, Zhang et al. (13) specially design an atmospheric-pressure plasma jet array to treat the surface of SRHTV materials. In this way, the reactive particles in the plasma can accelerate the accumulation of hydrophobic molecules on the SRHTV surface and result in a hydrophobicity improvement of SRHTV materials with the increase of water contact angle (CA) to 120°. Ahmadizadeh et al. (14) fabricate a super hydrophobic surface of SRHTV materials by the plasma treatment method under CF4 atmosphere. After treatment, the roughness of the surface is increased and the surface fluorination is successfully implemented. The super hydrophobic surface with CA of 151.3° is obtained due to the combined action of surface fluorination and roughness increment. Vazirinasab et al. (15) use the atmospheric-pressure air plasma system to treat SRHTV materials and create a micro- and nano-structured surface roughness. The modified SRHTV materials show a super hydrophobic surface with 160° water CA. Although the aforementioned methods can be used to improve the hydrophobicity of SRHTV materials obviously, this equipment is high cost and inconvenient to use. Besides, the treatment efficiency is unsatisfied due to its small effective treatment area one time. So, it is not suitable for scale industrial applications currently. More crucial is that the etching method by plasma is also a kind of destruction to the surface of SRHTV materials and against the anti-aging performance subsequently. The anti-UV aging ability of SRHTV materials is another factor that influences their outdoor applications importantly (16). To enhance the anti-UV aging ability of SRHTV materials to avoid the formation of micro cracks, Zhang et al. (17) use nano TiO2 particles to fill the SRHTV matrix to prepare composite and use the UV radiation to evaluate its UV aging behavior. The results indicate the excellent physical properties and surface hardness stability of SRHTV materials after the introduction of nano TiO2 UV light stabilizer. Lei et al. (18) introduce the nano TiO2 particles onto the surface of SRHTV materials via the spray method to build the UV shielding layer. After the aging process, the cracked micro-surface, increased water absorption, and decreased mechanical property are dramatically improved compared with neat SRHTV materials. Mohammed et al. (19) found the effect of ZrO2 nanoparticles on the color stability of SRHTV materials by artificial aging. The results indicate that ZrO2 nanoparticles provide important protection and show a reduction in color change of SRHTV materials. In fact, the failure of SRHTV materials in outdoors is caused jointly by many factors, including hydrophobicity, UV radiation, and physical scratch. However, the existing literature is mainly focused on the single research of hydrophobicity improvement or anti-UV aging ability improvement or the research of aging mechanism (20,21,22). Therefore, it is significant to develop a kind of SRHTV materials with excellent hydrophobicity, anti-UV aging ability, and reparability simultaneously to avoid the performance deterioration due to the formation of micro cracks under harsh environment.

Based on the aforementioned analysis, the combination of surface roughness increment and the employment of the UV shielding agent is an effective method to achieve the aforementioned objectives. ZnO particle is an excellent UV absorbent that has a broad application in anti-UV fields and shows favorable results (23,24). Because the size of nano ZnO (nZ) is too small to build the rough surface, the three-dimensional tetrapod ZnO (tZ) whiskers with micron size is introduced onto the surface of SRHTV materials to construct a functional layer with hydrophobicity characteristic and anti-UV ability in this work. To achieve the steady distribution of tZnO whiskers on the surface, the room temperature vulcanized silicone rubber (SRRTV) is used as the bonding layer between the SRHTV matrix and the ZnO functional layer. As an auxiliary, a bit of nZnO particles is added into the bonding layer to fill the gaps between tZnO whiskers on the surface. Besides, the bis(triethoxysilylpropyl) disulfide (Si75) is employed in the bonding layer to increase its reparability due to the reconfigurable disulfide bond. In a word, in this work, nZnO, tZnO, and Si75 are complementarily combined and introduced onto the surface of SRHTV materials by the dip-coating method using SRRTV as a bonding layer. The composition and microstructure on the effect of hydrophobicity for prepared SRHTV materials are researched, and the content of Si75 on the thermal-reparability of bonding layer is assessed. The water CA, mechanical property, and thermo gravimetric (TG) analysis of prepared SRHTV materials are studied after longtime accelerated UV aging process, and the SEM, FTIR, UV-vis DRS, and X-ray diffraction (XRD) analysis are used to analyze the mechanism.

2 Materials and methods

2.1 Materials

The SRHTV product is purchased from Wenzhou Ruwei Electric Co., Ltd (Wenzhou, China). The SRRTV is purchased from Hebei Zhonglian Huayu Electric Power Technology Co., Ltd (Handan, China). The analytical reagent ethyl acetate is purchased from Sinopharm Chemical Reagent Co., Ltd (Shanghai, China). The nano-ZnO (nZ) with about 100 nm particle size and bis(triethoxysilylpropyl) disulfide (Si75) are purchased from Shanghai Aladdin Biochemical Technology Co., Ltd (Shanghai, China), and the tZ with about 40–60 µm whisker length is supplied by Chengdu Crystrealm Co., Ltd (Chengdu, China).

2.2 Preparation

The modification of SRHTV is prepared by the following steps. First, the SRHTV materials are ultrasonic cleaned to remove the dust, greasy dirt, and unsteady fillers on the surface. Then the SRRTV, Si75, nZnO, and tZnO with different mass ratio are mixed to prepare a homogeneous mixture with 50 wt% concentration using ethyl acetate as a solvent. At the same time, the ready SRHTV is dipped into the pre-prepared mixture. Subsequently, the varnished SRHTV is pulled out and left at room temperature for 60 min to evaporate the solvent. Then, the functional mixture underwent accelerated curing under 60°C for 6 h to obtain the hydrophobic-UV shielding functional layer on the surface of SRHTV materials. During the preparation process, the content of SRRTV is maintained as constant. The content of Si75 is changed from 1 to 20% and that for nZnO is 1 to 7% and for tZnO is 10 to 50%. By this method, the prepared materials are marked as x-Si75/y-nZ/z-tZ@SR, and here, the x, y, and z stand for the contents of Si75, nZnO, and tZnO relative to SRRTV, respectively. The simulated diagram of the preparation process is shown in Figure 1.

Figure 1 Simulated diagram of the preparation process for Si75/nZ/tZ@SRHTV materials.
Figure 1

Simulated diagram of the preparation process for Si75/nZ/tZ@SRHTV materials.

2.3 Experiments

2.3.1 Ultraviolet aging experiment

The UV aging test of different Si75/nZ/tZ@SRHTV materials is performed in a UV aging test chamber (ZN-P, Wuxi Yierda Test Equipment Manufacturing Co., Ltd, China) under 40°C and 280–320 nm UV radiation for uninterrupted 0, 100, 200, 300, and 400 h, respectively.

2.3.2 Thermal repairing experiment

First, the incision is cut on the Si75/nZ/tZ@SRHTV materials throughout the functional layer and the matrix layer. Then, the materials are put into the constant temperature oven (DHG-9240A, China) under 80°C for 4 h.

2.3.3 Scanning electron microscopy (SEM) analysis

The microstructures of the surface for neat SRHTV and the prepared Si75/nZ/tZ@SRHTV materials before and after UV aging radiation are observed by the SEM (Hitachi TM3030, Japan).

2.3.4 CA analysis

The hydrophobicity of neat SRHTV and the prepared Si75/nZ/tZ@SRHTV materials before and after UV aging radiation is tested by CA meter (DSA100, Germany).

2.3.5 Mechanical property

The mechanical properties of neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials before and after UV aging radiation are measured by electronic universal testing machine (Instron 5969, USA).

2.3.6 TG analysis

The thermostability of neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials before and after UV aging radiation is measured by TG analyzer (Discovery TGA 550, America) in a nitrogen atmosphere. The test temperature range is room temperature to 750°C, and the heating rate is 10°C/min.

2.3.7 Fourier-transform infrared (FTIR) spectroscopy analysis

The structure of neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials before and after UV aging is tested by Fourier-transform infrared spectroscopy (Bruker Vertex 70, Germany). The scanning range is 400–4,000 cm−1, and the scanning rate is 20 min−1.

2.3.8 XRD analysis

The crystal structure of neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials before and after UV aging radiation is analyzed by X-ray diffractometer (Rigaku SmartLab SE, Japan) at room temperature. The test range of diffraction angle 2θ is 5–90°.

2.3.9 UV-visible diffuse reflectance spectroscopy (UV-vis DRS) analysis

The performance of UV light response for neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials is analyzed by UV-visible diffuse reflectance spectroscopy (PE lambda 750, America) with the test range of 200–800 nm wavelengths.

3 Results and discussion

3.1 Microstructure of Si75/nZ/tZ@SRHTV materials before UV aging

The microstructures of 10-Si75/y-nZ/50-tZ@SRHTV materials with different nZnO contents are observed as shown in Figure 2. A rough surface can be observed in Figure 2a with 1% content of nZnO, and this surface is no longer rough enough with the gradual increase of nZnO content in the bonding layer. This phenomenon can be explained by the following reasons probably. The nZnO particles are dispersed evenly in the SRRTV bonding layer and the viscosity of the matrix is greatly increased. Then, this high-viscosity mixture is tightly adhered to the tZnO whiskers and makes the surface smooth and dense relatively.

Figure 2 Microstructure of Si75/nZ/tZ@SRHTV with different nZnO contents before UV aging. (a) Microstructure with 1% nZnO, (b) microstructure with 3% nZnO, and (c) microstructure with 7% nZnO.
Figure 2

Microstructure of Si75/nZ/tZ@SRHTV with different nZnO contents before UV aging. (a) Microstructure with 1% nZnO, (b) microstructure with 3% nZnO, and (c) microstructure with 7% nZnO.

The microstructures of 10-Si75/1-nZ/z-tZ@SRHTV materials with different contents of tZnO whiskers are further observed as shown in Figure 3. It can be clearly seen that the rough surface is formed after the introduction of big-size tZnO whiskers (Figure 3a). With the increase of the tZnO content gradually, the promotion of surface roughness becomes visible (Figure 3b–d), especially the sample with 50% content of tZnO whiskers in Figure 3e. Understandably, this is the inevitable result due to the insertion and distribution of large amounts of tZnO whiskers on the bonding layer surface. The enlargement microstructure for Si75/nZ/tZ@SRHTV material with 50% content of tZnO whiskers is shown in Figure 3f. It is obvious that the partial region of tZnO whiskers is inserted into the bonding layer tightly and others are exposed. Besides, the nZnO particles can also be found on the gap surface of the bonding layer between tZnO whiskers. Through the combined function of this microstructure, the surface of Si75/nZ/tZ@SRHTV materials can be covered by ZnO UV absorbent.

Figure 3 Microstructure of Si75/nZ/tZ@SRHTV with different tZnO contents before UV aging. (a) Microstructure with 10% tZnO, (b) microstructure with 20% tZnO, (c) microstructure with 30% tZnO, (d) microstructure with 40% tZnO, (e) microstructure with 50% tZnO, and (f) enlargement of image.
Figure 3

Microstructure of Si75/nZ/tZ@SRHTV with different tZnO contents before UV aging. (a) Microstructure with 10% tZnO, (b) microstructure with 20% tZnO, (c) microstructure with 30% tZnO, (d) microstructure with 40% tZnO, (e) microstructure with 50% tZnO, and (f) enlargement of image.

The microstructures of neat SRHTV and the prepared x-Si75/1-nZ/50-tZ@SRHTV materials with different Si75 contents are observed by SEM as shown in Figure 4. A distinct morphology can be found between the neat SRHTV and the Si75/nZ/tZ@SRHTV materials. As to the neat SR, the surface shows flat and smooth microstructure, and some inorganic reinforced fillers are exposed on the surface (Figure 4a). Oppositely, a very rough surface with vast of tetrapod mastoids can be found for x-Si75/1-nZ/50-tZ@SRHTV materials. The formation of rough surface is due to the large number of ruleless distribution of tZ whiskers on the surface of the bonding layer. In addition, many big pores can be found on the surface of x-Si75/1-nZ/50-tZ@SRHTV materials, which are formed due to the curing shrinkage of the bonding layer and also because of the solvent evaporation. This special morphology and structure are beneficial to hold the air and are in favor of the improvement of water CA. Among the x-Si75/1-nZ/50-tZ@SRHTV materials within the 1–10% content of Si75, their microstructures are similar without an evident difference as shown in Figure 4b–f. However, with the further increase of the Si75 content, a sparse tZnO distribution and visibly reduced roughness can be observed in Figure 4g when the Si75 content exceeds 20%. Thus, it can be concluded that 10% Si75 is the suitable content to obtain a favorable rough surface. Moreover, the microstructure of cross section for 10-Si75/1-nZ/50-tZ@SRHTV material is observed as shown in Figure 4i, and the bottom SRHTV matrix containing large amount of inorganic fillers can be found obviously. The middle bonding layer SRRTV is adhered to the SRHTV matrix tightly, and the phase separation phenomenon is hardly happened due to the similar chemical structure between SRRTV and SRHTV. According to the scale, the thickness of the middle bonding layer is about 34 μm. Besides, the tZ whiskers are uniformly distributed on the outside of bonding layer and abundant bramble texture is formed, which can build the hydrophobic layer and UV shielding layer.

Figure 4 Microstructure of Si75/nZ/tZ@SRHTV with different Si75 contents before UV aging. (a) Microstructure of neat SRHTV, (b) microstructure with 1% Si75, (c) microstructure with 3% Si75, (d) microstructure with 5% Si75, (e) microstructure with 7% Si75, (f) microstructure with 10% Si75, (g) microstructure with 20% Si75, (h) enlargement of image (f), and (i) cross section microstructure of image (f).
Figure 4

Microstructure of Si75/nZ/tZ@SRHTV with different Si75 contents before UV aging. (a) Microstructure of neat SRHTV, (b) microstructure with 1% Si75, (c) microstructure with 3% Si75, (d) microstructure with 5% Si75, (e) microstructure with 7% Si75, (f) microstructure with 10% Si75, (g) microstructure with 20% Si75, (h) enlargement of image (f), and (i) cross section microstructure of image (f).

The thermo-reparability of Si75/nZ/tZ@SRHTV materials with different Si75 contents is evaluated by the SEM microstructure analysis. As shown in Figure 5a and b, the very remarkable incision still existed after thermal treatment. Perhaps, its Si75 content is too low and cannot play the repairing role. With the increase of the Si75 content to 5–7%, the incised faults are gradually repaired (Figure 5c and d). And with the further increase of Si75 content to 10–20%, the incised faults are nearly repaired as shown in Figure 5e and f due to the excellent molecular remodeling the ability of S–S bond of Si75 in the bonding layer. The favorable reparability can be obviously observed in the polymer matrix from the enlarged microstructures in Figure 5g and h. The cross-section microstructure of Si75/nZ/tZ@SRHTV materials with 10% content of Si75 is also observed as shown in Figure 5i, and it can be clearly seen that the incised fault of the bottom SRHTV matrix is unrepaired, while that of the surface layer is well repaired. The results indicated that the sufficient content of Si75 is benefited from the thermo-reparability, and 10% Si75 is the suitable content for the Si75/nZ/tZ@SRHTV materials with good thermo-reparability.

Figure 5 Repaired microstructure of Si75/nZ/tZ@SRHTV after thermal treatment. (a) Microstructure with 1% Si75, (b) microstructure with 3% Si75, (c) microstructure with 5% Si75, (d) microstructure with 7% Si75, (e) microstructure with 10% Si75, (f) microstructure with 20% Si75, (g) enlargement of image (e), (h) enlargement of image (f), and (i) cross section microstructure of image (e).
Figure 5

Repaired microstructure of Si75/nZ/tZ@SRHTV after thermal treatment. (a) Microstructure with 1% Si75, (b) microstructure with 3% Si75, (c) microstructure with 5% Si75, (d) microstructure with 7% Si75, (e) microstructure with 10% Si75, (f) microstructure with 20% Si75, (g) enlargement of image (e), (h) enlargement of image (f), and (i) cross section microstructure of image (e).

3.2 Hydrophobicity of Si75/nZ/tZ@SRHTV materials before UV aging

The hydrophobicity of prepared Si75/nZ/tZ@SRHTV materials can be represented by its water CA. To get a Si75/nZ/tZ@SRHTV material with excellent hydrophobicity, the content of Si75, nano ZnO, and tZ is researched on the effect of hydrophobicity. It can be clearly seen from Figure 6 that the hydrophobicity of Si75/nZ/tZ@SRHTV materials is dramatically affected by its component content. The hydrophobicity of neat SRHTV material is inferior with just 112.0° CA. But that for Si75/nZ/tZ@SRHTV materials is markedly improved, and its water CA even can reach to 151.2°. The notable improvement of hydrophobicity is likely attributed to the formation of the rough surface after the introduction of tZnO. However, the introduction of nZnO is unbeneficial to the improvement of hydrophobicity for Si75/nZ/tZ@SRHTV materials. And its CA is decreased with the increase of the nZnO content as shown in Figure 6a. This change is consistent with that of the rough surface in Figure 2. In consideration of the positive uvioresistant function of nZnO on the SRRTV bonding layer, the 1% content of nZnO can be considered as a suitable dosage with not particularly great impact on the hydrophobicity of Si75/nZ/tZ@SRHTV materials. The effect of the tZnO content on the hydrophobicity of Si75/nZ/tZ@SRHTV materials is further studied as shown in Figure 6b. The introduction of the low content of tZnO shows no evident improvement in its hydrophobicity until 40% percentage, and its CA tends to be stable at 50% tZnO content. So, 50% tZnO is considered the suitable content. As to the Si75, with the increase of its content from 0 to 20%, the CA of Si75/nZ/tZ@SRHTV materials decreases gradually from 151.2° to 122.0°. Perhaps, the decrease of CA is caused by the reduction of the relative amount ratio of tZnO whiskers due to the excess addition of Si75. In view of the equal importance of hydrophobicity and the thermo-reparability in Figure 5 for Si75/nZ/tZ@SRHTV materials, the 10% percentage of Si75 can be considered as the preferred content. Thus, the optimal content of this material is 10% Si75, 1% nZnO, and 50% tZnO and the corresponding material is marked as 10-Si75/1-nZ/50-tZ@SRHTV.

Figure 6 CA of Si75/nZ/tZ@SRHTV materials with different contents of nZnO (a), tZnO (b), and Si75 (c).
Figure 6

CA of Si75/nZ/tZ@SRHTV materials with different contents of nZnO (a), tZnO (b), and Si75 (c).

3.3 Microstructure of Si75/nZ/tZ@SRHTV materials after UV aging

The digital photo of the apparent color for Si75/nZ/tZ@SRHTV materials with different tZnO contents after UV aging is shown in Figure 7a. The Si75/nZ/tZ@SRHTV materials with low content of tZnO whiskers show a deep yellow surface layer, and this apparent color becomes shallow with an increase of the tZnO content. Finally, the apparent color changes to white when the content of tZnO exceeds 40%. The yellowing surface is associated with the change of microstructure. Thus, the SEM is used to observe the microtopography. The distinct breakages can be found on the surface when the content of tZnO is within 10–30% range which indicates the poor anti-UV performance. And the microstructure of Si75/nZ/tZ@SRHTV materials is almost the same as that of no UV aging in Figure 3 when the content of tZnO exceeds than 40%. This phenomenon is consistent with that of apparent color. The results can verify that the high content of tZnO distributed on the outermost layer of Si75/nZ/tZ@SRHTV materials is beneficial to its anti-UV aging performance.

Figure 7 Apparent color and microstructure of Si75/nZ/tZ@SRHTV materials with different tZnO contents after 400 h UV aging. (a) Apparent colour with tZnO content. (b) Microstructure with 10% tZnO content. (c) Microstructure with 20% tZnO content. (d) Microstructure with 30% tZnO content. (e) Microstructure with 40% tZnO content. (f) Microstructure with 50% tZnO content.
Figure 7

Apparent color and microstructure of Si75/nZ/tZ@SRHTV materials with different tZnO contents after 400 h UV aging. (a) Apparent colour with tZnO content. (b) Microstructure with 10% tZnO content. (c) Microstructure with 20% tZnO content. (d) Microstructure with 30% tZnO content. (e) Microstructure with 40% tZnO content. (f) Microstructure with 50% tZnO content.

Similarly, the digital photo of the apparent color for Si75/nZ/tZ@SRHTV materials with different Si75 contents after UV aging is shown in Figure 8a. It can be clearly seen that the color of the functional layer changes from white to brown gradually with the increase of the Si75 content in Si75/nZ/tZ@SRHTV materials, especially when the content of Si75 exceeds 10%. The microstructure of these Si75/nZ/tZ@SRHTV materials is also observed by SEM image. Different with the morphology shown in Figure 8a, many shocking breakages and flaking pieces occur on the surface of neat SRHTV materials due to its poor anti-UV performance. In contrast, the Si75/nZ/tZ@SRHTV materials present well anti-UV performance and intact surface morphology Figure 8b–g, and these microstructures are hardly changed compared with that of no UV aging. However, with the further increase of the Si75 content, the shocking breakages and flaking pieces are observed again on the surface when the Si75 content exceeds 20% as shown in Figure 8h and i. The variation tendency of microstructure observed by SEM is consistent with that of apparent color. It can be concluded that the 10% content of Si75 is the suitable dosage for the preparation of Si75/nZ/tZ@SRHTV materials with good hydrophobicity and anti-UV aging ability.

Figure 8 Apparent color and microstructure of Si75/nZ/tZ@SRHTV materials with different Si75 contents after 400 h UV aging. (a) Apparent colour with different Si75 content. (b) Microstructure of neat SRHTV. (c) Microstructure with 1% Si75 content. (d) Microstructure with 3% Si75 content. (e) Microstructure with 5% Si75 content. (f) Microstructure with 7% Si75 content. (g) Microstructure with 10% Si75 content. (h) Microstructure with 20% Si75 content. (i) Enlargement of image (h).
Figure 8

Apparent color and microstructure of Si75/nZ/tZ@SRHTV materials with different Si75 contents after 400 h UV aging. (a) Apparent colour with different Si75 content. (b) Microstructure of neat SRHTV. (c) Microstructure with 1% Si75 content. (d) Microstructure with 3% Si75 content. (e) Microstructure with 5% Si75 content. (f) Microstructure with 7% Si75 content. (g) Microstructure with 10% Si75 content. (h) Microstructure with 20% Si75 content. (i) Enlargement of image (h).

3.4 Hydrophobicity of Si75/nZ/tZ@SRHTV materials after UV aging

The water CA of neat SRHTV and Si75/nZ/tZ@SRHTV materials with different Si75 content after different UV aging time is tested and shown in Figure 9. The CA for all SRHTV samples is decreased gradually with the prolongation of UV aging time to 400 h. Among which, the neat SRHTV shows the highest strength drops especially, and its CA decreases to 84.82% level of the initial value. The deterioration of hydrophobicity is caused by the surface hardening and breakage. As a contrast, the CA of Si75/nZ/tZ@SRHTV materials keeps relatively stable with a lower declining rate after UV aging. Their CAs are still maintained at 92.33–98.02% level of initial value with a slight decrease of water CAs. The results illustrate that the prepared Si75/nZ/tZ@SRHTV materials possess an excellent anti-UV aging performance.

Figure 9 CA of Si75/nZ/tZ@SRHTV materials after different UV aging time.
Figure 9

CA of Si75/nZ/tZ@SRHTV materials after different UV aging time.

3.5 Mechanical property of Si75/nZ/tZ@SRHTV materials

The mechanical property of neat SRHTV and Si75/nZ/tZ@SRHTV materials at different UV aging stage is researched as shown in the stress–strain curve in Figure 10. It is obvious that the breaking strength of Si75/nZ/tZ@SRHTV materials is a little higher than that of neat SRHTV materials before any UV aging time. Perhaps, it can be attributed to the physical crosslinking function of a large amount of ZnO inorganic particles in the bonding layer. With the prolongation of UV aging time, the deterioration of mechanical properties for neat SRHTV materials is increasingly obvious, especially the samples after 400 h longtime UV aging with significantly reduced breaking strength and elongation at break. In contrast, the variation of mechanical properties is not very obvious for Si75/nZ/tZ@SRHTV materials after UV aging, and its breaking strength is always higher than that of neat SRHTV materials under the same UV aging time. The deterioration of mechanical property is caused by the breakage of molecular chains of SRHTV materials under UV radiation. The results fully demonstrate the good anti-UV aging ability of prepared Si75/nZ/tZ@SRHTV materials and also indicate the potential applicability.

Figure 10 Stress–strain curves of Si75/nZ/tZ@SRHTV materials after different UV aging time.
Figure 10

Stress–strain curves of Si75/nZ/tZ@SRHTV materials after different UV aging time.

3.6 Thermostability of Si75/nZ/tZ@SRHTV materials

The thermostability of neat SRHTV and Si75/nZ/tZ@SRHTV materials before and after 400 h UV aging is researched by the TG analysis, and the results are shown in Figure 11. The thermo-gravimetric curves in Figure 11a show that the mass residual rate of neat SRHTV materials is about 67.3%, but that of Si75/nZ/tZ@SRHTV is lower than neat SRHTV materials whatever UV aged or not. It is because of the high content of inorganic fillers contained in neat SRHTV materials. And the content of ZnO particles introduced in the bonding layer is lower than that of the original fillers. Compared with the sample before UV aging, the mass residual rate of Si75/nZ/tZ@SRHTV materials hardly changed after UV aging, but that of neat SRHTV materials present a clearly visible change with an increased mass residual rate after UV aging. It may be due to the break off of aged SRHTV polymer and much more exposure to inorganic particles on the surface. The DTG curves are further studied as shown in Figure 11b. It can be seen that the thermostability of Si75/nZ/tZ@SRHTV materials is better than that of neat SRHTV materials with high initial decomposition temperature (T initial), maximum degradation rate temperature (T max), and end decomposition temperature (T end). It is because the large number of inorganic ZnO whiskers are concentrated on the surface and can promote the thermostability of Si75/nZ/tZ@SRHTV materials to a certain degree.

Figure 11 TG analysis of Si75/nZ/tZ@SRHTV materials. TG curves (a) and DTG curves (b).
Figure 11

TG analysis of Si75/nZ/tZ@SRHTV materials. TG curves (a) and DTG curves (b).

3.7 FTIR structure of Si75/nZ/tZ@SRHTV materials

The structure of neat SRHTV and Si75/nZ/tZ@SRHTV materials before and after UV aging is determined and shown in Figure 12. Many characteristic absorption peaks (25) can be observed from Figure 12a. The absorption peak at 786.77 cm−1 belonged to the groups of Si–(CH3)2, and the peaks at 1,005.26 and 1,258.32 cm−1 belonged to Si–O–Si and Si–CH3, respectively. Compared with the neat SRHTV materials, some new absorption peaks can be found in the FTIR spectra, among which the peak at 464.36 cm−1 belonged to Zn–O, the peak at 1,082.86 cm−1 belonged to the S–C bond, and the peak at 1,538.72 cm−1 belonged to terminal O–H groups in polymethylethylsiloxane molecular chains. After the 400 h UV aging, the absorption peak intensity of Si–(CH3)2 (Figure 12b), Si–O–Si (Figure 12c), and Si–CH3 (Figure 12d) for neat SRHTV materials shows an evident decrease. It is because that the energy of UV radiation is strong enough and can cut off the groups of Si–CH3 and Si–O–Si. On the contrast, the intensity of these absorption peaks hardly changed for Si75/nZ/tZ@SRHTV materials after UV aging. The results indicate that the aging reaction occurred easily on the surface of neat SRHTV materials after being exposed to UV radiation for a long time and also illustrate the excellent anti-UV aging ability of prepared Si75/nZ/tZ@SRHTV materials again.

Figure 12 ATR mode FTIR spectra of Si75/nZ/tZ@SRHTV materials before and after UV aging.
Figure 12

ATR mode FTIR spectra of Si75/nZ/tZ@SRHTV materials before and after UV aging.

3.8 XRD analysis of Si75/nZ/tZ@SRHTV materials

The XRD spectra of Si75/nZ/tZ@SRHTV materials with different Si75 contents before and after UV aging are tested and shown in Figure 13. As to the neat SRHTV materials before UV aging, some obvious diffraction peaks at 2θ = 20.61°, 26.35°, 36.30°, 45.51°, 49.88°, 54.71°, 59.72°, and 67.98° can be observed. Because of the amorphous characteristic of hydroxy-terminated polymethylethylsiloxane for the main component of neat SRHTV materials, these diffraction peaks belonged to the crystal structure of inorganic fillers in SRHTV materials, such as Fe2O3, Al(OH)3, and SiO2. After 400 h longtime UV aging, these diffraction peaks still existed, and no new peak can be discovered. But the intensities of these diffraction peaks are significantly enhanced. This enhancement shows that the high contents of inorganic fillers are exposed on the surface due to the breakage of polymer for neat SRHTV materials after UV aging. This inference can also be verified by the SEM observation. In contrast, the XRD patterns of Si75/nZ/tZ@SRHTV materials are different from that of neat SRHTV materials. A large number of diffraction peaks for ZnO crystal (26) can be observed at 2θ = 31.53°, 34.24°, 36.02°, 47.29°, 56.33°, and 62.59°, instead of that for inorganic fillers in SRHTV materials. And with the increase of the Si75 content and the relative decrees of the ZnO content, these diffraction peak intensities get weaken gradually. The characteristic peak at 2θ = 26.35° even can be observed for the Si75/nZ/tZ@SRHTV sample with a high content of Si75 like 20-Si75/1-nZ/50-tZ@SRHTV material. As to these Si75/nZ/tZ@SRHTV materials, the XRD patterns remain keep almost unchanged after UV aging. The results indicate that Si75/nZ/tZ@SRHTV materials possess excellent anti-UV aging ability. However, as to the 20-Si75/1-nZ/50-tZ@SRHTV material, the diffraction peaks belonging to the inorganic fillers at 2θ = 49.88°, 54.71°, and 59.72° appeared after 400 h UV aging. Perhaps, the inorganic fillers are exposed and can be detected from the crack fissure for 20-Si75/1-nZ/50-tZ@SRHTV material after UV aging. The results show that the high content of Si75 is unfavorable for the UV stability of Si75/nZ/tZ@SRHTV materials.

Figure 13 XRD patterns of Si75/nZ/tZ@SRHTV materials before and after UV aging.
Figure 13

XRD patterns of Si75/nZ/tZ@SRHTV materials before and after UV aging.

3.9 UV-visible diffuse reflection analysis of Si75/nZ/tZ@SRHTV materials

The neat SRHTV and prepared Si75/nZ/tZ@SRHTV materials with different Si75 contents are tested by UV-vis DRS to evaluate their photoresponse characteristics, including the UV radiation and visible radiation. The spectrogram is shown in Figure 14. It can be clearly seen that the neat SRHTV shows very low reflectance on UV radiation and partially visible radiation within the 200–550 nm region. The low reflectance means high absorption of optical radiation. And the result indicates that the neat SRHTV material has a strong absorption of UV radiation and partial visible light. By contrast, the reflectance on UV radiation decreases a little for Si75/nZ/tZ@SRHTV materials due to the strong absorption of ZnO particles on UV radiation. However, ZnO particles distributed on the surface of Si75/nZ/tZ@SRHTV materials have no response to visible light, and these materials show very high reflectance on visible radiation. With the increase of Si75 content, the reflectance on UV radiation is almost unchanged. But at the visible light region, the reflectance of Si75/nZ/tZ@SRHTV materials is decreased gradually. Low content of Si75 means a high content of tZnO relatively. Thus, the Si75/nZ/tZ@SRHTV materials with low content of Si75 show high reflectance on visible radiation due to their strong diffuse reflection and scattering. Therefore, it can be concluded that the prepared Si75/nZ/tZ@SRHTV materials have a good resistance to light radiation.

Figure 14 UV-visible diffuse reflection spectra of Si75/nZ/tZ@SRHTV materials.
Figure 14

UV-visible diffuse reflection spectra of Si75/nZ/tZ@SRHTV materials.

3.10 Mechanism analysis of Si75/nZ/tZ@SRHTV materials

Based on the aforementioned experiment results and analysis, the possible mechanism for prepared Si75/nZ/tZ@SRHTV materials is explored shown in Figure 14. As mentioned earlier, the surface of neat SRHTV materials is relatively smooth and some inorganic fillers are exposed on the surface, which leads to the hydrophilic nature. The moisture is easily condensed and adhered to the surface, which will cause accidents and accelerate the aging reaction. At the same time, the mainly absorbed UV radiation by SRHTV materials matrix will further aggravate the aging reaction. Conversely, the rough functional layer is formed on the surface of SRHTV materials by the introduction and distribution of ZnO whiskers with excellent UV shielding ability. The moisture droplet is difficult to adhere to the surface. And the UV shielding layer constructed by nZnO/tZnO can effectively absorb the UV radiation and can also enhance the diffuse reflection of solar radiation. In addition, the evenly distributed Si75 in the bonding layer can play the molecular remodeling function and repair the scratches or cracks. Under the combined action of aforementioned factors, the stability of SRHTV materials will be promoted dramatically in outdoors application. The mechanism is simulated as shown in Figure 15.

Figure 15 Stabilization mechanism simulation of Si75/nZ/tZ@SRHTV materials. (a) Hydrophobicity, (b) anti-UV ability, and (c) thermal-reparability.
Figure 15

Stabilization mechanism simulation of Si75/nZ/tZ@SRHTV materials. (a) Hydrophobicity, (b) anti-UV ability, and (c) thermal-reparability.

4 Conclusions

To promote the property and expand the application of SRHTV materials, a functional layer is introduced on the surface of SRHTV materials by the dip-coating method to prepare a series of Si75/nZ/tZ@SRHTV materials. The hydrophobicity and microstructure are researched to optimize the content of functional additives such as Si75, nZnO, and tZnO. The uninterrupted 400 h accelerated UV radiation is used to evaluate the anti-UV aging ability of Si75/nZ/tZ@SRHTV materials. It is found that the SRRTV bonding layer can steadily and tightly adhere to the surface of the SRHTV matrix after curing and presents favorable interfacial compatibility due to their similar molecular chain structure and chemical characteristics. The tZnO whiskers can distribute on the surface of SRHTV randomly to form a uniformly rough surface layer and build a bramble mastoid structure on the outside. At the same time, the nZnO particles can evenly disperse in the matrix of the SRRTV bonding layer and can fill the gap surface of the bonding layer between tZnO whiskers. The surface roughness of Si75/nZ/tZ@SRHTV materials is promoted gradually with the increase of the tZnO content due to the greater distribution of three-dimensional long whiskers, and its water CA also shows the same tendency. On the contrast, the introduction of nZnO particles plays an opposite effect. In addition, the combined utilization of nZnO and tZnO can cover the whole surface of the bonding layer and endow the Si75/nZ/tZ@SRHTV materials with the excellent anti-UV ability. After the 400 h UV aging, the surface of neat SRHTV shows typical aging characteristic with obvious cracks while that for Si75/nZ/tZ@SRHTV materials are still intact at high content of tZnO whiskers. The introduction of Si75 dilutes the real content of tZnO whiskers and shows disadvantage to the improvement of water CA and also the anti-UV aging ability. Its CA is decreased, and the yellowed apparent surface is formed and many shocking breakages are observed on the microstructure with the increasing Si75 content. But on the other hand, the existence of Si75 can play as a consolidant and endow the Si75/nZ/tZ@SRHTV materials a good reparability after thermal treatment at suitable Si75 content due to its reconfigurable disulfide bond. The 10-Si75/1-nZ/50-tZ@SRHTV can be considered as the material with optimal performance in consideration of the hydrophobicity and anti-UV ability and thermal-reparability. After the longtime accelerated UV radiation, the Si75/nZ/tZ@SRHTV materials still shows a good hydrophobicity and intact surface morphology and also a good mechanical property compared with the neat SRHTV materials. The FTIR analysis indicates the breakage of Si–O molecular chains of neat SRHTV by UV radiation with an evident decrease of the intensity of Si–(CH3)2, Si–O–Si, and Si–CH3, while that for Si75/nZ/tZ@SRHTV materials is hardly changed. The XRD analysis indicates the exposure of inorganic fillers for neat SRHTV with increased diffraction peak intensities after UV aging, while that for Si75/nZ/tZ@SRHTV materials is unchanged. With the further increase of Si75 content exceeding than 10%, some small diffraction peaks belonging to the inorganic fillers in SRHTV matrix appeared after UV aging. This phenomenon is consistent with its microstructure. Besides, the TG results show that the thermostability of Si75/nZ/tZ@SRHTV materials is better than that of neat SRHTV materials with increased T initial, T max, and T end due to the introduction of the amount of inorganic tZnO whiskers. The research indicates that the prepared Si75/nZ/tZ@SRHTV materials by the dip-coating method in this work possess excellent comprehensive performance.

  1. Funding information: The author states no funding involved.

  2. Author contribution: Zhaohua Zhang: data curation, methodology, investigation, writing.

  3. Conflict of interest: The author states no conflict of interest.

  4. Data availability statement: The authors confirm that the data and materials supporting the findings of this study are available within the article.

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Received: 2024-08-03
Revised: 2024-09-12
Accepted: 2024-09-14
Published Online: 2024-11-19

© 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/epoly-2024-0079
Keywords for this article
silicone rubber; hydrophobicity; anti-UV ability; thermal-reparability; dip-coating method
Creative Commons
BY 4.0

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  39. Experimental study on impact and flexural behaviors of CFRP/aluminum-honeycomb sandwich panel
  40. Normal-hexane treatment on PET-based waste fiber depolymerization process
  41. Effect of tannic acid chelating treatment on thermo-oxidative aging property of natural rubber
  42. Design, synthesis, and characterization of novel copolymer gel particles for water-plugging applications
  43. Influence of 1,1′-Azobis(cyclohexanezonitrile) on the thermo-oxidative aging performance of diolefin elastomers
  44. Characteristics of cellulose nanofibril films prepared by liquid- and gas-phase esterification processes
  45. Investigation on the biaxial stretching deformation mechanism of PA6 film based on finite element method
  46. Simultaneous effects of temperature and backbone length on static and dynamic properties of high-density polyethylene-1-butene copolymer melt: Equilibrium molecular dynamics approach
  47. Research on microscopic structure–activity relationship of AP particle–matrix interface in HTPB propellant
  48. Three-layered films enable efficient passive radiation cooling of buildings
  49. Electrospun nanofibers membranes of La(OH)3/PAN as a versatile adsorbent for fluoride remediation: Performance and mechanisms
  50. Preparation and characterization of biodegradable polyester fibers enhanced with antibacterial and antiviral organic composites
  51. Preparation of hydrophobic silicone rubber composite insulators and the research of anti-aging performance
  52. Surface modification of sepiolite and its application in one-component silicone potting adhesive
  53. Study on hydrophobicity and aging characteristics of epoxy resin modified with nano-MgO
  54. Optimization of baffle’s height in an asymmetric twin-screw extruder using the response surface model
  55. Effect of surface treatment of nickel-coated graphite on conductive rubber
  56. Experimental investigation on low-velocity impact and compression after impact behaviors of GFRP laminates with steel mesh reinforced
  57. Development and characterization of acetylated and acetylated surface-modified tapioca starches as a carrier material for linalool
  58. Investigation of the compaction density of electromagnetic moulding of poly(ether-ketone-ketone) polymer powder
  59. Experimental investigation on low-velocity-impact and post-impact-tension behaviors of GFRP T-joints after hydrothermal aging
  60. The repeated low-velocity impact response and damage accumulation of shape memory alloy hybrid composite laminates
  61. Exploring a new method for high-performance TPSiV preparation through innovative Si–H/Pt curing system in VSR/TPU blends
  62. Large-scale production of highly responsive, stretchable, and conductive wrapped yarns for wearable strain sensors
  63. Preparation of natural raw rubber and silica/NR composites with low generation heat through aqueous silane flocculation
  64. Molecular dynamics simulation of the interaction between polybutylene terephthalate and A3 during thermal-oxidative aging
  65. Crashworthiness of GFRP/aluminum hybrid square tubes under quasi-static compression and single/repeated impact
  66. Review Articles
  67. Recent advancements in multinuclear early transition metal catalysts for olefin polymerization through cooperative effects
  68. Impact of ionic liquids on the thermal properties of polymer composites
  69. Recent progress in properties and application of antibacterial food packaging materials based on polyvinyl alcohol
  70. Additive manufacturing (3D printing) technologies for fiber-reinforced polymer composite materials: A review on fabrication methods and process parameters
  71. Rapid Communication
  72. Design, synthesis, characterization, and adsorption capacities of novel superabsorbent polymers derived from poly (potato starch xanthate-graft-acrylamide)
  73. Special Issue: Biodegradable and bio-based polymers: Green approaches (Guest Editors: Kumaran Subramanian, A. Wilson Santhosh Kumar, and Venkatajothi Ramarao)
  74. Development of smart core–shell nanoparticles-based sensors for diagnostics of salivary alpha-amylase in biomedical and forensics
  75. Thermoplastic-polymer matrix composite of banana/betel nut husk fiber reinforcement: Physico-mechanical properties evaluation
  76. Special Issue: Electrospun Functional Materials
  77. Electrospun polyacrylonitrile/regenerated cellulose/citral nanofibers as active food packagings
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