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Effect of surface treatment of nickel-coated graphite on conductive rubber

  • Xindi Zhuang EMAIL logo , Baotong Xing , Hongda Mao , Wei Liu and Hua Zou EMAIL logo
Published/Copyright: December 3, 2024
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e-Polymers
From the journal e-Polymers Volume 24 Issue 1

Abstract

In the blended conductive rubbers, good dispersion of conductive fillers and great interfacial bonding with the substrate are the keys to achieving excellent mechanical and electromagnetic shielding properties. It is found that compared with octyltriethoxysilane (A137), 3-methacryloxypropyl-trimethoxysilane (A174) and vinyltriethoxysilane (A151) with a double bond reduce the curing degree of the blends. The vinyl methyl silicone rubber/nickel-coated graphite (VMQ/NCG) composites modified by A137 shows poor tensile properties, while the composites modified by A174 shows inferior electrical properties. The presence of physical adsorption and chemical adsorption on the surface of NCG modified by A151, which effectively enhances the dispersibility of NCG and interfacial bonding strength with rubber, so that the material exhibits excellent comprehensive properties. When the content of A151 is 3% and modified by dry method, the tensile strength of VMQ/NCG composites can reach 1.6 MPa, the elongation at break can reach 162%, and the volume resistivity can reach 0.05 Ω·cm.

Keywords: silicone rubber; nickel-coated graphite; coupling agent; conductive rubber; Soxhlet extraction

1 Introduction

Conductive silicone composites, including conductive fillers and silicone rubber, have unique characteristics such as excellent high- and low-temperature resistance, aging resistance, processability, and electrical conductivity. When used in aerospace systems, electronic chips, and other systems, they exhibit electromagnetic sealing characteristics, preventing important information leakage (1–5). Common conductive fillers include carbon (6–12) and metal fillers (13–15). Carbon fillers are generally more suitable for the preparation of conductive rubber with low conductivity. Although metal fillers have good electrical conductivity, they have high price and density. Conductive polymers often require the addition of dopants to achieve good shielding properties, which leads to relatively poor processability and mechanical properties, so they are also used as conductive fillers (16). Nowadays, it has become a new trend to adopt composite conductive fillers (17–20) with low density, good conductivity, aging resistance, and moderate cost, and to mix different conductive fillers (21–23). Among them, nickel-coated graphite (NCG) has good electrical conductivity and magnetic permeability. Moreover, silicone conductive materials with NCG, which can effectively prevent electromagnetic leakage or shield external electromagnetic interference, are widely used (24–26). However, NCG, which is an inorganic filler, has a high surface energy and hydrophilic surface, resulting in poor compatibility with rubber matrix. This causes NCG agglomeration, reduces the amount of NCG used to form conductive networks, and causes NCG direct filled silicone rubber to exhibit poor mechanical properties; hence, the surface modification of NCG is indispensable.

Silane coupling agents are first used to treat glass fiber, a reinforcing agent used in plastics. Modification using silane coupling agents is an environmentally friendly, simple, and low-cost method (27). Silane coupling agents have an organic group at one end that can be chemically bonded to a polymer or exhibit good compatibility with the polymer, and an alkoxy group at the other end. The alkoxy group of silane coupling agents is hydrolyzed, forming a silanol group, which establishes a hydrogen bond with the hydroxyl group on the surface of an inorganic material and forms a covalent bond between the coupling agent and inorganic material after dehydration. Alternatively, the alkoxy group of silane coupling agents directly condenses with the hydroxyl group on the surface of an inorganic material to form a covalent bond with the inorganic material, replacing the original van der Waals forces. Furthermore, the organic group at the other end of the coupling agent is bonded to the rubber, thereby enhancing the interfacial adhesion between the inorganic material and rubber (28). This also reduces the surface energy of the inorganic materials and the filler–filler interaction, reducing the agglomeration phenomenon, improving the filler dispersion, and effectively enhancing the performance of the composite material (29). Currently, the application of silane coupling agents has gradually extended to surface modification of nanoparticles such as silica and metal oxides, and many studies have investigated the interaction between the coupling agents and nanoparticles and discussed their effects on the properties of obtained composites (30–33). However, fewer studies examined the interaction between silane coupling agents and composite metal fillers as well as their effect on the properties of conductive rubber.

Herein, we studied the possible use of coupling agents to modify NCG and the effect of the type and loading of coupling agents as well as the treatment technique, including dry method pretreatment, wet method pretreatment, and in situ treatment (IST), on the morphology, curing characteristics, tensile properties, and electrical conductivity of silicone rubber composites filled with NCG. In addition, X-ray photoelectron spectroscopy (XPS) was used to characterize the untreated and treated NCG surfaces, which clarified the modification mechanism and provided basis for developing conductive rubber with high electromagnetic shielding characteristics and excellent tensile properties.

2 Materials and methods

2.1 Materials

Vinyl methyl silicone (VMQ) rubber (Grade KE931-U) was acquired from Shin-Etsu Chemical, Japan. NCG (average particle size of 100 μm and nickel content of 60%) was supplied by Novamet Corporation, USA. Bis (2,4-dichlorobenzoyl) peroxide (DCBP) was used as a curing agent and was obtained from Qiangsheng Chemical Engineering Company, Jiangsu, China. Vinyltriethoxysilane (A151), octyltriethoxysilane (A137), and 3-methacryloxypropyl-trimethoxysilane (A174) were used as silane coupling agents and were obtained from GE Toshiba Silicones Co., Ltd, Japan.

2.2 Surface treatment of NCG and preparation of VMQ/NCG composites

Two methods were used to pretreat the NCG powder using a silane coupling agent: dry method treatment (DMT) and wet method treatment (WMT). In DMT, a high-speed mixer was used to disperse pure silane coupling agent into the conductive filler. In WMT, A151, A137, or A174 was diluted with ethanol (water content = 0.5%) to a concentration of 5% and the weighed conductive fillers were then added to the silane coupling agent and ethanol mixture. Next, the mixture was stirred for 30 min and then heated in a water bath at 80°C until the ethanol solvent was completely volatilized. Finally, the treated conductive filler was baked in an air oven for 2 h at 120°C. The IST method involved sequential addition of conductive filler and coupling agent to the rubber followed by their mixing at 120°C without pretreatment.

The pretreated conductive filler was fully mixed with the rubber in a two-roll mill to provide a good dispersion of the filler without destroying the nickel coating, and then DCBP was added to the mixture to obtain the mixed rubber. The blends prepared using IST were cooled to room temperature (23℃), and DCBP was added into the masterbatch. The compositions used in this study are shown in Table 1. The mixed rubber was hot pressed at 112°C and 10 MPa for 10 min to complete the first stage of the curing reaction and then heat treated in a blast oven at 200°C for 2 h to complete the second stage of the curing reaction to obtain vulcanizates.

Table 1

Compositions of conductive silicone rubber

Ingredients phr
VMQ 100
NCG 200
DCBP 8
Coupling agent Variable

2.3 Characterization

2.3.1 Environmental scanning electron microscopy (ESEM)

The morphology of the NCG powder and VMQ/NCG composites were observed using an ESEM.

2.3.2 XPS

The XPS analyses of the untreated and treated NCG were conducted using an ESCALAB 250 spectrometer (Thermo-VG Scientific, UK) with an Al Kα X-ray (1,486.6 eV) source. Survey scan spectra were acquired at binding energies of 0–1,000 eV at a step of 1 eV to examine the elemental composition of the materials, and the atomic percentages were calculated based on these spectra. In addition, a narrow scan of silicon 2p (Si2p) spectra was obtained at 90–114 eV using a step of 0.1 eV.

2.3.3 Characterization of the curing parameters

An M-3000A rotorless rheometer (High-speed Railway Testing Instrument Co., Ltd, China) was used to detect the curing curve of the VMQ/NCG composites at 112°C. For the curing characteristic analysis, the curing parameters, such as minimum torque (M L) and maximum torque (M H), were obtained based on the curing curve. T 90 is defined as the optimal curing time, which is the time corresponding to the torque of M L + (M H − M L) × 90%, whereas T 10 is the time of scorching, which is the time corresponding to the torque of M L + (M H − M L) × 10% (34). The cure rate index (CRI) represents the curing speed of the silicone rubber and can be calculated as follows (34):

(1) CRI = 100 / ( T 90 − T 10 )

2.3.4 Rubber processing analysis

The relationship between the dynamic modulus G′ and strain of mixed rubber and that between tanδ and the strain of the vulcanizates were tested using an RPA2000 rubber processing analyzer (USA) at 60°C and 1 Hz.

2.3.5 Volume resistivity

A QJ84 (Shanghai Zhengyang Instrument Factory, China) micro-ohmmeter was used for volume resistivity testing in accordance with ASTM D991 by the four-probe method.

2.3.6 Tensile properties

The tensile properties were tested using a CMT4104 universal testing machine (Shenzhen SANS Group Company, China) at a speed of 500 mm·min−1 in accordance with ASTM D412.

3 Results and discussion

3.1 Effect of the type of silane coupling agent

Figure 1 shows the ESEM micrographs of the NCG packing. It can be seen from the figure that the NCG particles are irregular flaky (Figure 1a), with an average particle size of 100 μm. The nickel coating is flat, dense, and completely encapsulates the graphite core. A very small part of the graphite core is not completely covered by the nickel coating, and the defects exist on the flat part of the graphite surface rather than at both ends (Figure 1b).

Figure 1 ESEM micrographs of the NCG filler.
Figure 1

ESEM micrographs of the NCG filler.

As shown in Figure 2a, the untreated VMQ/NCG composites exhibits the highest M L, reflecting its relatively high viscosity (35). The M L of the VMQ/NCG composite decreases after the surface treatment, indicating a decrease in the viscosity and an increase in the dispersion of the NCG in the rubber matrix (Figure 2b). The ΔM (M H−M L) of the A137 sample is slightly smaller than the untreated sample, but it exhibits a smaller curing rate. It is worth noting that the ΔM and curing rate of A174 and A151 samples are smaller than the untreated sample and the A174 sample is the smallest. The probable reason is that the C═C bond of the coupling agent consumes the DCBP. Under the initiation of DCBP, the coupling agent produces free radicals that can be used for self-polymerization of coupling agent molecules or grafted to the molecular chain of VMQ, resulting in a reduced amount of free radicals used for rubber cross-linking, and exhibiting a smaller curing degree and curing rate. Moreover, compared to A151, the polar double bond of A174 has a higher activity (36) and consumes more DCBP, thus the A174 sample exhibits minimal curing degree and curing rate.

Figure 2 (a) Curing characteristic curves of the VMQ/NCG composite and (b) comparison of NCG dispersion before and after coupling-agent modification.
Figure 2

(a) Curing characteristic curves of the VMQ/NCG composite and (b) comparison of NCG dispersion before and after coupling-agent modification.

The tensile properties and conductive properties of the VMQ/NCG composites are shown in Figure 3. The untreated sample exhibits a minimum tensile strength and a maximum volume resistivity. After the surface treatment of NCG, the tensile strength of VMQ/NCG composites is improved and corresponds to their ∆M. Among them, the A137 sample exhibits the smallest elongation at break, while the A174 sample shows the highest elongation at break. Specifically, the tensile strength and elongation at break of the A151 sample are 1.2 MPa and 162%, respectively, representing an increase of 50% and 63% with the untreated sample. Moreover, the volume resistivity is 0.06 Ω·cm, which is reduced by 80%. The A151 sample exhibits a faster curing rate, the best conductivity, and moderate tensile properties, so it is the optimal surface-modification agent among the three coupling agents.

Figure 3 (a) Tensile properties and (b) conductive properties of the VMQ/NCG composite.
Figure 3

(a) Tensile properties and (b) conductive properties of the VMQ/NCG composite.

The ESEM images of the untreated VMQ/NCG sample and the A151 sample are shown in Figure 4. Numerous holes are observed on the fractured section of the untreated VMQ/NCG sample, indicating a weak interaction between the NCG powder and VMQ. No obvious holes are observed on the fractured section of the A151-modified sample, indicating that A151 improves the interaction between the NCG powder and VMQ.

Figure 4 ESEM micrographs of the VMQ/NCG composites (a) without A151 and (b) with A151.
Figure 4

ESEM micrographs of the VMQ/NCG composites (a) without A151 and (b) with A151.

3.2 Effect of the A151 content

The curing, mechanical, and conductive characteristics of the VMQ filled with NCG treated using different A151 content are listed in Table 2. With increasing A151 content, ΔM gradually decreases, indicating a decrease in the curing density of the rubber matrix (37). Moreover, with the increase of A151 content, the scorch time remains unchanged, and A151 consumes DCBP, which reduces the free radical amount during the crosslinking process of VMQ (38), thus slowing down the curing rate, showing an increase in the optimal curing time and a decrease in CRI. The tensile strength of all samples increases upon increasing the A151 content from 1% (given in mass ratio based on NCG) to 3% and decreases when the A151 content is approximately 4%. The maximum tensile strength is observed at an A151 content of 3%. Moreover, the volume resistivity of all samples decreases with the increase in the A151 content from 1% to 3% and increases at approximately 4%.

Table 2

Effect of A151 content on the properties of VMQ/NCG composites

Content of A151 (%) 1 2 3 4
Min torque M L (dN·m) 7.35 6.65 7.15 6.85
Max torque M H (dN·m) 25.66 22.49 21.25 18.52
M H − M L (dN·m) 18.31 15.48 14.10 11.67
Scorch time T 10 (min) 0.30 0.30 0.32 0.31
Optimum curing time T 90 (min) 13.5 17.0 18.7 38.0
CRI (min−1) 7.6 6.0 5.4 2.7
Volume resistivity (Ω·cm) 0.21 0.13 0.09 0.50
Tensile strength (MPa) 1.12 1.34 1.82 0.89
Stress at 50% elongation (MPa) 0.90 1.04 1.35 0.53
Elongation at break (%) 159 121 75 102

These phenomena can be attributed to two factors. The dispersion of the NCG in the rubber matrix and the filler–rubber interaction are improved with increasing A151 content, enhancing the tensile strength and conductivity of the VMQ/NCG composite (Factor I). However, the curing density of the rubber matrix decreases with increasing A151 content, leading to an increased volume resistivity and decreased tensile strength (Factor II). At an A151 content lower than 3%, the effect of Factor I on the properties of the composites is greater than that of Factor II; thus, the tensile strength and conductivity increase with the increase in the A151 content. However, when the A151 content reaches 4%, the effect of Factor II is more prominent, leading to a decrease in the curing density, a reduction in the tensile strength, and an increase in the volume resistivity. Therefore, the optimal A151 content is 3%.

3.3 Effect of filler treatment techniques

Different treatment techniques have different effects on the rubber properties. Thus, three different treatments, namely WMT, DMT, and IST, were studied. Figure 5a shows the curing curve of the VMQ/NCG composite treated using different techniques. The ΔM of the WMT sample is higher than those of the samples treated using the other two treatment techniques, suggesting that the WMT-treated VMQ/NCG composite has the highest curing level.

Figure 5 (a) Curing curves and (b) tanδ–strain curve of the VMQ/NCG composites treated by different techniques, (c) G′–strain curve of mixed rubber, and (d) stress–strain relationship of the VMQ/NCG composites treated using different techniques.
Figure 5

(a) Curing curves and (b) tanδ–strain curve of the VMQ/NCG composites treated by different techniques, (c) G′–strain curve of mixed rubber, and (d) stress–strain relationship of the VMQ/NCG composites treated using different techniques.

The loss factor (tanδ)–strain curves of VMQ/NCG composites obtained by the three different treatment methods are shown in Figure 5b. Although the WMT sample exhibits the highest curing degree, it has the highest tanδ, indicating that the energy dissipation and heat accumulation in the rubber composites are pronounced under cyclic loading conditions, reflecting weak filler–matrix interaction and/or agglomeration of some of the filler (39). According to Figure 5c, with the increase in the strain, the storage modulus of VMQ/NCG composites considerably decreases, showing an obvious Payne effect. The decrease value of G′ (∆G) in the G′–strain curve can be used to evaluate the strength of the filler network in the rubber (24). The larger the ∆G is, the stronger the filler network is (40,41). The filler network includes the interaction between the filler–filler and the interaction between the filler–rubber (42). The ∆G of the WMT sample is smaller than that of the other two samples (Figure 5c), indicating that the filler network of the VMQ/NCG composites treated with WMT is weak, i.e., the weak filler–filler interaction and/or weak filler–rubber interaction. The stress–strain curve of the WMT sample exhibits a yield point phenomenon (Figure 5d), indicating an improvement of the dispersion of the filler without agglomeration after the WMT treatment. Moreover, this phenomenon is combined with a larger tanδ and a smaller ∆G, indicating that the interfacial filler–rubber interaction is weaker than those of the samples treated with the other two methods.

The tensile properties of the samples treated using different techniques are shown in Figure 5d and conductive properties of the samples are shown in Figure 6. The WMT sample exhibits the lowest tensile strength and hardness as well as the highest elongation. Meanwhile, the WMT sample exhibits the largest volume resistivity, indicating the lowest conductivity among all treated samples. The IST sample exhibits the highest tensile strength and hardness as well as the lowest elongation. The DMT sample exhibits moderate hardness and excellent tensile properties. The IST and DMT samples exhibit similar conductivities, which is in good agreement with the results illustrated in Figure 5c. Compared with CHO-SEAL® 6371, the tensile strength and elongation at break of the DMT sample increase by 53% and 62%, respectively, and the volume resistivity decreases by 50%. DMT can improve the mechanical and electrical properties of rubber, exhibits easy implementation, high production efficiency, and easy real-time monitoring of modified quality; thus, it has potential application in the rubber industry (43).

Figure 6 Shore A hardness and conductive properties of the VMQ/NCG composites treated using different techniques.
Figure 6

Shore A hardness and conductive properties of the VMQ/NCG composites treated using different techniques.

3.4 Modification mechanism of A151 on the NCG powder

The A151-modified NCG pretreated using WMT is considered as an example to examine the mechanism of the A151-modified NCG. Three samples were studied to examine the surface-modification mechanism of the NCG by A151. Unmodified NCG powder is designated Sample 1#. Surface-modified NCG powder with 10% A151 pretreated using WMT is labeled Sample 2#. To prepare Sample 3#, some of Sample 2# is Soxhlet-extracted by ethanol, which is a good solvent for A151, for 24 h. After the Soxhlet extraction, the sample is air dried at 100°C for 4 h. Ni, O, and C can be detected on the surfaces of all three samples, whereas Si is only observed on the surface of Samples 2# and 3# (Figure 7). The results reveal that A151 can successfully modify the surface of NCG after WMT. After 24 h of Soxhlet extraction, physical adsorption is no longer observed on the surface of NCG, leaving only chemical adsorption (44). Table 3 provides detailed information corresponding to Figure 7a. The Si2p content in Samples 1#, 2#, and 3# are 0%, 14.94%, and 9.27%, respectively. Compared with Sample 2#, the decrease in the Si2p content in Sample 3# indicates the presence of physical and chemical adsorptions between A151 and NCG, of which chemical adsorption accounts for a large part.

Figure 7 (a) XPS spectra and (b) Si 2p spectra of the composites.
Figure 7

(a) XPS spectra and (b) Si 2p spectra of the composites.

Table 3

Content of different surface elements in Samples 1#, 2#, and 3#

1# 2# 3#
C1s (%) 55.71 45.34 59.11
O1s (%) 33.14 34.47 27.85
Ni2p (%) 11.15 5.24 3.76
Si2p (%) — 14.94 9.27
Si/Ni (ration) 0 2.85 2.47

The A151 monomer dissolved in ethanol during the WMT evaporates during the volatilization of ethanol. Thus, no A151 monomer is bound to the of NCG surface with van der Waals forces. Owing to the slow rate of hydrolysis of siloxanes under neutral conditions, the alkoxy group of A151 is not completely hydrolyzed (32,45). Oligomers can be formed by a dehydration condensation reaction between the hydroxyl groups of partially hydrolyzed A151 monomers (46). The surface treatment layer of NCG pretreated with WMT may contain the following types of physical adsorption: attachment of the A151 oligomers to the surface through van der Waals forces (Figure 8a) and attachment of the A151 monomers to the surface through hydrogen bonds (Figure 8b). In addition, A151 monomers (Figure 8c) and A151 oligomers (Figure 8d) are bound to the surface via covalent bonds.

Figure 8 Mechanism of the A151-modified NCG.
Figure 8

Mechanism of the A151-modified NCG.

4 Conclusions

Herein, the effect of the surface treatment of NCG on the properties of conductive silicone rubber and the interaction between coupling agents and NCG were investigated. A151, the best modifier among the studied modifiers (A151, A137, and A174), can improve the dispersion of the filler in the rubber matrix and the interfacial bond strength between the silicone rubber and NCG. The results of Soxhlet extraction combined with XPS indicate that A151 is bound to the NCG surface through physical and chemical adsorptions, in which chemical adsorption plays the major role. The optimal A151 content, at which the best overall performance is obtained, is found to be 3%. The filler treatment exhibits a considerable effect on the rubber properties. Among the tested techniques, DMT is simple to operate and has transparent quality control process. In addition, it considerably improves the mechanical properties of the composite. Thus, it exhibits excellent potential for industrial production.

Abbreviations

A137

octyltriethoxysilane

A151

vinyltriethoxysilane

A174

3-methacryloxypropyl-trimethoxysilane

DCBP

bis (2,4-dichlorobenzoyl) peroxide

DMT

dry method treatment

IST

in situ treatment

NCG

nickel-coated graphite

WMT

wet method treatment

Acknowledgements

The authors thank the Ministry of Education Fund for sponsoring this study.

  1. Funding information: This work was funded by the Ministry of Education Fund (No. 8091B012104).

  2. Author contributions: Xindi Zhuang: investigation, writing – original draft; Hua Zou: methodology, resources, supervision; Baotong Xing: formal analysis, experimental data processing; Wei Liu: writing – review and editing, visualization; Hongda Mao: writing – review and editing, formal analysis.

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

  4. Data availability statement: The data that support the findings of this study may be provided by the corresponding authors upon reasonable request.

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Received: 2024-04-18
Revised: 2024-07-04
Accepted: 2024-07-07
Published Online: 2024-12-03

© 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-2024-0045
Keywords for this article
silicone rubber; nickel-coated graphite; coupling agent; conductive rubber; Soxhlet extraction
Creative Commons
BY 4.0

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