Influence of mica paper surface modification on the water resistance of mica paper/organic silicone resin composites

Haisheng Wang; Heyi Ge; Junke Xu

doi:10.1515/secm-2024-0023

Article Open Access

Influence of mica paper surface modification on the water resistance of mica paper/organic silicone resin composites

Haisheng Wang , Heyi Ge and Junke Xu

Published/Copyright: August 22, 2024

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From the journal Science and Engineering of Composite Materials Volume 31 Issue 1

Abstract

This study enhances the water resistance of mica paper/organic silicone resin composites through surface modification with 3-aminopropyltriethoxysilane (APTES). The Fourier-transform infrared spectroscopy and the X-ray photoelectron spectroscopy confirmed the formation of chemical bonds between APTES and mica. The results showed that at an optimal APTES concentration of 0.6%, the water diffusion coefficient decreased from 5.0 × 10⁻³ mm²/min to 2.7 × 10⁻³ mm²/min, and the permeability coefficient decreased from 5.71 × 10⁻⁴ mm²/min to 1.94 × 10⁻⁴ mm²/min, with a significant reduction in equilibrium water uptake. Additionally, the modified composites exhibited minimal mechanical strength loss after moisture aging, demonstrating excellent water resistance. The interface shear strength tests revealed a 28.6% increase in interfacial bonding strength after APTES modification. This study demonstrates the potential of silane coupling agents to enhance the performance of inorganic polymer composites, providing theoretical support for their industrial application.

Keywords: mica; silicone resin; 3-aminopropyltriethoxysilane; surface modification; water resistance

1 Introduction

Mica is a unique type of sheet silicate mineral primarily composed of SiO₂, containing elements such as lithium, potassium, aluminum, iron, and magnesium [1,2,3]. Its crystalline structure, consisting of two layers of tetrahedral silicon–oxygen sandwiching an octahedral layer of aluminum–oxygen, bestows it with exceptional electrical insulation properties and chemical stability, even at high temperatures [4,5]. Common types of mica include muscovite, biotite, and synthetic mica, with the general chemical formula KAl₂(AlSi₃O₁₀)(OH)₂. Mica paper is produced from natural or synthetic mica that is ground into fine particles. This powder is then suspended in water to form a slurry, spread on a screen, and dried to create continuous sheets of mica paper [6,7]. The formation mechanism of mica paper is due to the attractive forces between the parallel planes of mica flakes, which results in the paper’s lower mechanical strength and interface performance, as well as its limited workability [7]. To enhance its mechanical properties, mica paper typically requires the use of adhesives to bond it with reinforcing materials. Mica paper/silicone resin composite materials are composed of mica paper and silicone resin adhesives. The silicone resin is evenly applied to the mica paper, which after drying and thermal pressing, results in a sturdy laminated board [8]. This mica laminate is crucial in the electrothermal appliance industry, capable of long-term usage at temperatures up to 1,000°C. It exhibits good bend strength and workability, and its toughness allows it to be processed into various shapes without delaminating. It is widely used in industries such as metallurgy, chemical, and household appliances, for products like hair dryers, soldering irons, and heating coils [9,10,11]. However, the relatively low surface energy of mica paper affects the wetting properties of resins on its surface [12]. Good wetting is essential for forming uniform coatings, and low surface energy prevents resins from spreading evenly on mica paper, thereby affecting its bonding performance. Additionally, the chemical inertness of mica paper makes it difficult to form stable chemical bonds with resins [13,14,15]. Due to the poor interfacial compatibility between mica and silicone resin, the composite material is highly susceptible to moisture in the air. Water molecules infiltrate and accumulate along the microvoids and cracks at the interface, further expanding these defects. This ultimately leads to the degradation of the interfacial structure, significantly reducing the mechanical strength of the material and adversely affecting the long-term durability and service life of the composite [16,17,18]. To improve compatibility between mica paper and resins, surface treatments such as roughening and chemical modification are often necessary to enhance the bonding strength between them [6,19]. There are many methods to improve the interface bonding quality between inorganic and organic materials [15,20–23], physical coating modification, and mechanical force chemical modification. Among these, surface chemical modification proves effective in enhancing interface adhesion quality between resins and inorganic materials, currently being the most widely used method for inorganic material modification [24–26]. For instance, Chen et al. [27] utilized silane coupling agents and titanium salts to modify mica, investigating the impact on polypropylene (PP) performance. The results revealed that 3-methacryloxypropyltrimethoxysilane modification improved bending and tensile performance of composites, 3-methacryloxypropyltrimethoxysilane and JN-114 enhanced toughness of PP composites, and different modified micas as mineral fillers generated synergistic effects with PP. Xiao et al. [28] employed silane coupling agents such as 3-Aminopropyltriethoxysilane (APTES), 3-glycidoxypropyltrimethoxysilane, and 3-methacryloxypropyltrimethoxysilane to modify sericite and investigated the impact of this modification on the performance of polyimide composites. The results demonstrated that APTEX-modified sericite exhibited the strongest interfacial bonding with polyimide, resulting in superior mechanical and thermal properties in the composites and the lowest dielectric constant. He et al. [29] modified ramie fibers using amino silicone oil, transforming the surface from hydrophilic to hydrophobic, thereby enhancing interface compatibility and improving mechanical performance of composites.

This study introduces a method for enhancing the interfacial adhesion and water resistance of mica paper/organic silicone resin composites through the surface chemical modification of mica paper using APTES. The research focuses on the interfacial behavior and reinforcement mechanisms of the composites, evaluating the impact of moisture absorption on the interfacial properties of the composites before and after modification. By systematically studying the effects of different APTES concentrations on composite performance, the optimal modification concentration was determined. Additionally, this study examines the performance of the composites not only in humid environments but also under mechanical stress conditions. Through the combination of moisture absorption experiments and theoretical calculations, the specific mechanisms by which moisture uptake affects the properties of the composites are elucidated. This research method not only validates the experimental results but also provides theoretical guidance for further optimization.

2 Experimental method

2.1 Materials

Methyl silicone resin DH-1 (Figure 1a) was provided by Jilin Donghu Organic Silicone Co., Ltd., Jilin, China. Mica paper (Figure 1b) and curing agent K-1 were supplied by Mica Electric Apparatus Co., Ltd., Guangdong, China. APTES was obtained from Nanjing Shuguang Chemical Group Co., Ltd., Nangjing, China. Deionized water was prepared in the laboratory, and methanol was of industrial grade.

Figure 1

(a) Methyl silicone resin. (b) Mica paper.

2.2 Preparation of organic silicone resin adhesive

The organic silicone resin adhesive was formulated by mixing methanol, DH-1, and K-1 in a specific ratio, followed by thorough mixing. The mixture was set aside for later use. The process is shown in Figure 2a.

Figure 2

(a) Preparation of methyl silicone adhesive. (b) Mica paper grafted APTES. (c) Preparation of mica paper/silicone resin composite.

2.3 Surface graft modification of mica paper

Initially, prepare a solution of APTES with a mass fraction of 5% by mixing methanol, deionized water, and APTES in a ratio of 80:15:5. Stir the mixture thoroughly and allow it to hydrolyze for 2 h. Then, apply the APTES solution of varying weights onto the surface of mica paper and dry it in a 100°C oven for 1 min. The process is shown in Figure 2b.

2.4 Preparation of APTES-mica paper/organic silicone resin composites

The mass ratio of resin adhesive to mica was calculated and controlled at 10:90. The organic silicone resin adhesive was coated onto the surface of APTES-modified mica paper. The adhesive-coated mica paper was dried in a 100°C oven. The adhesive-coated mica paper was neatly stacked into ten layers and subjected to heat pressing treatment in a hot press. The press was preheated to 250°C, and after inserting the adhesive-coated paper, a vacuum was drawn. The pressure was then raised to 10 MPa, and the heat press was maintained for 30 min. The process is shown in Figure 2c (Table 1).

Table 1

Abbreviations for samples

Samples	Annotate
P-Mica	Primordial mica
S-Mica	Surface treated mica
M/SC-1	Primordial mica paper/silicone composite
M/SC-2	0.2% APTES-mica paper/silicone composite
M/SC-3	0.4% APTES-mica paper/silicone composite
M/SC-4	0.6% APTES-mica paper/silicone composite
M/SC-5	0.8% APTES-mica paper/silicone composite

2.5 Characterization

Nicolet 380 Fourier-transform infrared spectroscopy (FTIR) was used to analyze attenuated total reflection spectra before and after surface treatment. The testing range was 400–4,000 cm⁻¹ with a resolution of 4 cm⁻¹. X-ray photoelectron spectroscopy (ESCALAB 250XI) was employed to study the functional group composition of the mica surface before and after treatment. A scanning electron microscope (FEI QUANTA 250 FEG) was used to observe the surface morphology of mica before and after surface treatment, as well as the microstructure of composites’ cross-sections. Water absorption rate testing was conducted according to ISO62-2008 standards. Mechanical properties were evaluated using an electronic universal testing machine (QJ-211) following GB/T1449-2005 standards. According to the JC/T 773-2010 standard, the interfacial shear strength (IFSS) between mica and resin was characterized, and IFSS was calculated using the following equation:

(2.1) IFSS = 3 4 × F b h ,

where IFSS represents the interfacial shear strength (MPa), F is the maximum load, b is the sample width (mm), and h is the sample thickness (mm).

3 Results and discussion

In Figure 3a and b, the infrared spectra of mica samples before and after silane treatment are depicted. The spectra show characteristic peaks at 815 and 1,000 cm⁻¹, attributed to the symmetric and antisymmetric Si-O-Si stretching vibrations in mica, respectively. The peak at 3,450 cm⁻¹ indicates the hydroxyl group stretching vibrations on the mica surface, while the peak at 1,631 cm⁻¹ is associated with water adsorption. After treatment, a new, broad, and weak absorption peak at 3,425 cm⁻¹ signals the introduction of C–N bonds due to the silane coupling agent. Additionally, the S-Mica samples exhibit distinct new peaks at 2,850 and 2,920 cm⁻¹, ascribed to the stretching vibrations of the alkyl chains from the silane agent.

Figure 3

(a) and (b) FT-IR spectra of P-Mica and S-Mica. (c) XPS spectra of P-Mica and S-Mica. (d) N1s XPS spectra of P-Mica and S-Mica.

X-ray photoelectron spectroscopy (XPS) analysis, as shown in Figure 3c and d, reveals the chemical structural modifications in mica induced by the treatment process. In the N(1s) spectra, the S-Mica samples display discernible nitrogen peaks, suggesting the successful grafting of amino groups from the silane coupling agent, unlike the P-Mica, where such features are absent. Notably, the N(1s) spectrum of S-Mica exhibits two distinct peaks associated with different nitrogenous states – protonated and non-protonated amines. The appearance of protonated amine signals is likely due to the interaction of NH/NH₂ groups from the agent with mica’s surface hydroxyls, leading to the formation of NH⁺/NH²⁺ species [30]. These spectral signatures substantiate the efficacy of the silane treatment in altering the mica’s surface chemistry [31].

Inorganic materials typically exhibit polar hydrophilic characteristics, whereas organic resins are generally nonpolar. This polarity mismatch poses a challenge in forming strong molecular bonds. Silane coupling agents are employed to enhance the bonding compatibility between these materials by altering the surface characteristics of inorganic substrates, as shown in Figure 4a. Post-modification with APTES, the mica surface becomes hydrophobic due to the introduction of organic functional groups, which is evidenced by the increased contact angle from 11.5° to 99.5°, indicating a significant increase in hydrophobicity. Furthermore, APTES reacts with the mica surface to form siloxane bonds, producing a thin siloxane film. This film contributes to an increased micro-roughness on the mica surface, leading to smaller water droplet contact angles and enhanced hydrophobicity, as detailed in Figure 4b.

Figure 4

(a) Contact angle measurements of mica paper. (b) Surface roughness measurement of mica paper.

Figure 5 showcases the microstructural contrasts between the composites. From the images, it can be observed that the structure of M/SC-1 is relatively loose, with noticeable voids at the interface between the mica paper and the resin, some of which can reach sizes of 200–300 μm, and there are many such voids. In contrast, the structure of M/SC-4 is more compact, with significantly smaller pore diameters and a reduced number of voids. The voids in the composite serve as channels that facilitate the diffusion of water molecules, causing expansion stress during moisture absorption. This may lead to cracking around the matrix area, and if the stress exceeds the interfacial bonding strength, it may result in mica detachment. Therefore, the hygroscopicity of M/SC-1 is mainly due to the voids in the composite, while the resin matrix has a smaller impact on the material’s moisture absorption.

Figure 5

Microstructure of composites.

The equilibrium water absorption rates and times of the mica paper/organic silicone resin composites immersed in distilled water at 25°C are detailed in Table 2. Following the application of the silane coupling agent, a decrease in the equilibrium water absorption rate is observed, reaching a minimum before subsequently increasing across the composite series from M/SC-1 to M/SC-4. The lowest absorption rate recorded is 7.20% for M/SC-1, with a corresponding increase in the time taken to reach water saturation from 17 to 23 days. The inherent differences in the properties of mica and organic silicone resin contribute to suboptimal resin penetration, resulting in interface voids. These voids, along with microcracks, facilitate the ingress and accumulation of water due to its small size and high polarity [32]. The silane treatment improves the interfacial bonding, effectively reducing these defects and enhancing the material’s resistance to water.

Table 2

Equilibrium water absorption rate and equilibrium water absorption time of mica paper/silicone composites

Samples	Equilibrium water absorption rate/%	Equilibrium water absorption time/day
M/SC-1	11.41	17
M/SC-2	9.78	19
M/SC-3	8.00	22
M/SC-4	7.20	23
M/SC-5	8.61	22

The absorption behavior of the resin-based composites can be described by Fick’s second law.

(3.1) M t M ∞ = 1 − 8 π 2 ∑ n = 0 ∞ 1 ( 2 n = 1 ) 2 exp − D ( 2 n + 1 ) 2 π 2 t h 2 ,

where M t represents the water absorption at time t, M ∞ represents the saturated water absorption, h is the sample thickness, and D is the diffusion coefficient. In the initial stage of moisture absorption behavior, the equation can be expressed as follows:

(3.2) M t M ∞ = 4 π 1 / 2 D t h 2 1 / 2 .

The formula can be further expressed as follows:

(3.3) M t = k t 1 / 2 .

If M t − t 1 / 2 linear relationship exists, it is possible to conclude that the moisture absorption behavior of composites conforms to Fick’s second law [33]. The M t − t 1 / 2 curve of the composites is shown in Figure 6a. From the graph, it can be observed that M t − t 1 / 2 exhibits linear growth in the initial stages of moisture absorption, followed by a gradual deviation and reaching equilibrium. This is consistent with Fick diffusion behavior.

Figure 6

(a) The relationship curves of water absorption vs t ^1/2 for mica paper/silicone composites. (b) The relationship curves of water absorption vs t ^1/2 for mica paper/silicone composites.

The diffusion coefficient (D) characterizes the speed of water diffusion. A larger D value indicates faster diffusion, and weaker interfacial bonding of the composites. Converting the water absorption–time curve ( M t – t relationship) into the M t – t / h relationship curve allows for the calculation of the diffusion coefficient D x .

(3.4) D x = π 1 4 M co d M d t / h ,

where D x represents the diffusion coefficient, M represents the water absorption, M ∞ represents the equilibrium water absorption, t represents the water absorption time, and h represents the sample thickness.

The water absorption of the sample increases rapidly in the early soaking stage, then gradually slows down until reaching equilibrium. When plotting M t against t / h , the slope of the linear portion of the curve is denoted as d M d t / h , as shown in Figure 6b.

The diffusion coefficients (D values) for the composites, as depicted in Table 3, demonstrate an initial decline, reaching a nadir with the 0.6% silane coupling agent application, which yields a D value of 2.7 × 10⁻³ mm²/min. An increase in the diffusion coefficient is observed as the concentration of the silane coupling agent continues to rise. A lower diffusion coefficient is indicative of superior interfacial bonding between the matrix and the reinforcing material, which hinders the mobility of water molecules within the composite. The employment of silane coupling agents effectively enhances this interfacial bond, as evidenced by the varying D values.

Table 3

Diffusion coefficients for mica paper/silicone composites

Samples	d M t / d t 1 2 h ( mm 0.5 / min )	D x × 10 ‒ 3 / ( mm 2 / min )
M/SC-1	0.073	5.0
M/SC-2	0.055	4.4
M/SC-3	0.034	3.4
M/SC-4	0.025	2.7
M/SC-5	0.042	3.8

The absorption coefficient S can be obtained using equation

(3.5) S = X ∞ X p ,

where X ∞ represents the equilibrium water absorption, and X p represents the initial mass of the composites.

The permeability coefficient P is the product of the diffusion coefficient D and the absorption coefficient S.

(3.6) P = D S .

The permeability coefficient (P) quantifies the volume of water that permeates through a given cross-section of the sample per unit time, effectively illustrating the dynamics between water diffusion and absorption within the material. According to the data presented in Table 4, the use of silane coupling agents significantly impacts this property. Initially, the permeability coefficient decreases from 5.71 × 10⁻⁴ mm²/min to a minimum of 1.94 × 10⁻⁴ mm²/min as the silane coupling agent concentration reaches 0.6%. Beyond this point, the diffusion coefficient begins to increase again. This trend suggests that the composite’s resistance to water permeation is optimized at a 0.6% concentration of the silane coupling agent, demonstrating the agent’s effectiveness in enhancing the material’s barrier properties against moisture ingress.

Table 4

Permeability coefficients for mica paper/silicone composites

Samples	S	P × 10 ‒ 4 / ( mm 2 / min )
M/SC-1	0.1141	5.71
M/SC-2	0.0978	4.30
M/SC-3	0.0800	2.72
M/SC-4	0.0720	1.94
M/SC-5	0.0861	3.27

Interface shear strength is a critical metric for assessing the quality of the bond between mica and organic silicone resin. This property was evaluated using the short beam method, and the findings are presented in Figure 7a. After treatment with a silane coupling agent, the interface strength increased from 10.3 MPa for M/SC-1 to 11.4 MPa for M/SC-2. As the amount of silane-treated mica increased, so did the interface strength, reaching a peak of 13.25 MPa at a silane coupling agent mass fraction of 0.6%. These results clearly demonstrate that the addition of the silane coupling agent significantly enhances the bonding between mica and organic silicone resin.

Figure 7

(a) Interfacial shear strength for mica paper/silicone composites. (b) The bending strength changes of composites after saturation hygroscopic and (c) after 1,000 h in 85% RH, 85°C environment. (d) The tensile strength changes of composites after saturation hygroscopic and (e) after 1,000 h in 85% RH, 85°C environment.

Figure 7 illustrates the changes in mechanical properties of mica paper/organic silicone resin composites before and after moisture absorption. The experimental environment of saturated moisture absorption aging is 100% RH and 25°C, and the experimental environment of 1,000 h moist heat aging is 85% RH and 85°C. The APTES-modified mica composites exhibit superior flexural and tensile strengths compared to the original composites, highlighting the effectiveness of surface chemical modification. The introduction of APTES not only enhances the hydrophobicity of the mica surface but also creates an alkaline microenvironment, which promotes stronger bonding between the mica and the organic silicone resin. This chemical modification via the silane coupling agent significantly strengthens the interface, thereby enhancing the composite’s resilience to stress-induced damage during moisture absorption. Optimal mechanical performance is observed when the APTES treatment concentration is at 0.6%. Figure 7b and c detail the variations in flexural strength post-saturation moisture absorption and after 1,000 h of exposure to 85% RH and 85°C. Compared to M/SC-1, M/SC-4 shows a 27.6% increase in flexural strength (from 199 to 254 MPa). Following moisture exposure, the flexural strength of M/SC-1 decreases by 85.3% (from 199 to 32 MPa) and 34.1% (from 199 to 131 MPa), while M/SC-4 experiences reductions of 57.7% (from 254 to 112 MPa) and 14.9% (from 254 to 216 MPa). Similarly, the tensile strength trends depicted in Figure 7d and e show that after moisture absorption, M/SC-1 undergoes reductions of 85.9% (from 178 to 25 MPa) and 30.9% (from 178 to 123 MPa), whereas M/SC-4 shows reductions of 61.6% (from 216 to 83 MPa) and 18.1% (from 216 to 177 MPa). These enhancements result in composites that demonstrate improved water resistance.

4 Conclusion

This study significantly enhanced the interfacial adhesion and water resistance of mica paper/organic silicone resin composites through surface modification with APTES. The main conclusions are as follows:

FTIR and XPS analyses confirmed the formation of stable chemical bonds between APTES and mica. This chemical bond formation is key for improving interfacial adhesion.

The optimal concentration of APTES is 0.6%. At this concentration, the water diffusion coefficient decreased from 5.0 × 10⁻³mm²/min to 2.7 × 10⁻³mm²/min, and the permeability coefficient decreased from 5.71 × 10⁻⁴mm²/min to 1.94 × 10⁻⁴mm²/min, with a significant reduction in equilibrium water uptake. Additionally, the modified composites exhibited minimal mechanical strength loss after moisture aging, demonstrating excellent water resistance.

APTES modification significantly increased the interfacial shear strength of the composites, reaching a maximum of 13.25 MPa, a 28.6% improvement compared to unmodified materials. This enhancement indicates the effectiveness of APTES in improving interfacial bonding quality.

The modified composites exhibited excellent performance in both humid environments and under mechanical stress conditions. Moisture aging tests and mechanical tests under high humidity conditions showed that the reductions in flexural and tensile strengths of the modified composites were significantly reduced, greatly enhancing their durability. After 1,000 h of moisture aging, the reduction in flexural strength decreased from 34.1 to 14.9%, and the reduction in tensile strength decreased from 30.9 to 18.1%. After moisture absorption saturation, the reduction in flexural strength decreased from 85.3 to 57.7%, and the reduction in tensile strength decreased from 85.9 to 61.6%.

Overall, this study demonstrates the significant potential of APTES in enhancing the performance of mica paper/organic silicone resin composites, providing new methods and theoretical support for developing high-performance, durable composites. These findings not only help understand the interfacial behavior of composites but also provide important references for their practical applications in various industrial fields.

Funding information: The authors appreciate financial support from the Natural Science Foundation of Shandong, China (Grant No. ZR2020ME040).
Author contributions: All authors have accepted responsibility for the entire content of this manuscript and consented to its submission to the journal, reviewed all the results and approved the final version of the manuscript. HW: methodology, data curation, and writing – original draft. HG: conceptualization and writing – review and editing. JX: visualization, investigation.
Conflict of interest: Authors state no conflict of interest.
Data availability statement: The raw/processed data required to reproduce these findings cannot be shared at this time as the data also form part of an ongoing study.

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Received: 2024-04-22

Revised: 2024-06-07

Accepted: 2024-06-08

Published Online: 2024-08-22

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

Articles in the same Issue

https://doi.org/10.1515/secm-2024-0023

Keywords for this article

mica; silicone resin; 3-aminopropyltriethoxysilane; surface modification; water resistance

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BY 4.0