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Synergistic effect of carbon nanotubes in combination with magnesium hydroxide on the flame retardant poly(ethylene-co-vinyl acetate)

  • Hongyan Li EMAIL logo , Hongli Liu , Junwei Li , Sen Tao , Jing Li , Yajing Li and Po Li
Published/Copyright: August 27, 2014
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Science and Engineering of Composite Materials
From the journal Science and Engineering of Composite Materials Volume 23 Issue 1

Abstract

To investigate the synergistic effect of carbon nanotubes (CNTs) in combination with magnesium hydroxide (MH) on the flame retardant poly(ethylene-co-vinyl acetate) (EVA), a series of EVA-based composites filled with CNTs, MH, a mixture of MH and CNTs, and MH-modified CNTs (MH-CNTs) were prepared. Characterizations of the fillers and the composites were performed by transmission electron microscopy, X-ray diffraction, Raman spectroscopy, thermogravimetric analysis, and cone calorimetry. The results indicated that the presence of CNTs affected the size of the attaching MH, which was decreased to around 20 nm. MH also had an enlarged special surface area in the MH-CNTs. A synergism was found in the MH-CNTs on the thermal retardant EVA composites due to the interaction between MH and CNTs.

Keywords: carbon nanotubes; flame retardancy; magnesium hydroxide; poly(ethylene-co-vinyl acetate); synergistic effect

1 Introduction

Ethylene-vinyl acetate copolymer (EVA) is commonly used in many fields, such as construction and cable industry, as a material with excellent physical and chemical properties [1, 2]. However, EVA is easily flammable and emits a large amount of smoke and toxic gases while burning [3]. The most traditional flame retardants of EVA are halogen ones; however, this system would contribute to more air pollution. According to the European Environment Agency, the best-known direct impacts are related to ambient air pollution, poor water quality, and insufficient sanitation [4]. Therefore, developing halogen-free flame retardant polymeric materials with low emission of smoke and poisonous gases, instead of the halogen flame retardant systems, have become a potential trend [5].

The thermal oxidative degradation of EVA consists of two steps. (i) The first and most intense step is the degradation step, which occurs between 300°C and 400°C, wherein small fragments corresponding to the acetic acid mother molecule can be found. At the end of this step, charred layers are formed. (ii) The second step is the oxidation of the charred layers [3, 6, 7]. Magnesium hydroxide (MH) is a green halogen-free flame retardant. It is required to reduce the first degradation step of EVA and avoid fire hazards and reduce flammability; however, the high loading of MH results in agglomeration and decrease of the mechanical performance of the materials. To further improve the mechanical and flame retardant properties of the EVA matrix, it becomes interesting to introduce other synergistic additives.

The synergistic effects of two or three inorganic particles in a flame retardant polymer have been reported in many articles [8–12]. Especially, the synergistic effects of mixed MH and carbon nanotubes (CNTs) were studied, and the improved flame retardancy of EVA was also found [13].

Since the landmark paper by Iijima [14], large attention has been paid to CNTs, which consist of rolled-up graphene sheet built from sp2 carbon units because of its potential applications due to extraordinary physical, chemical, and mechanical properties [15–19]. Meanwhile, CNTs improved the thermal stability of polymers owing to their thermal conductivity and ability of free radical capture [20–23]. With regard to the flame retardancy of CNTs, Beyer [24] embedded CNTs into an EVA matrix to investigate the flame retardancy of EVA by using a cone calorimeter first. The results showed that the obtained charred layers were more compact than those in clay/EVA, and the flame retardancy of CNTs/EVA was also improved. Recently, it appears interesting to use CNTs at a low loading content to obtain materials with reduced flammability. In our previous works [25, 26], iron oxide (III) nanoparticles were obtained on the surface of the CNTs, and a synergistic effect on the thermal stability of the polymer was also found. The existence of CNTs decreased the size of oxide particles, and the chemical interaction between CNTs and oxides also brought synergistic effects in the thermal-resistant polymer matrix.

In this study, monodispersed MH-modified CNTs were prepared and embedded into an EVA matrix to obtain a flame retardant nanocomposite. The mechanical properties and flame retardancy of the nanocomposite were investigated, and the synergistic effect of CNTs in combination with MH on the flame retardant EVA was also studied.

2 Materials and methods

2.1 Materials

The EVA copolymer (ELVAX 440; vinyl acetate content, 25 wt%) was purchased from DuPont (USA). Carboxylic CNTs (carboxyl ratio, 2.31 wt%; purity, >95%; diameter, 20–40 nm; length, 1–2 μm) were purchased from Shenzhen Nanotech Port Co., Ltd. (China). All other reagents were of analytical grade, which were obtained from Jiangtian Chemistry (Tianjin Co., Ltd., China).

2.2 Preparation of MH-CNTs

Mg(NO3)2·6H2 O (2.56 g) was added into 50 ml of absolute ethanol and stirred until it was dissolved completely. This solution was added with 0.35 g of carboxylic CNTs, stirred, and sonicated for 1 h. The solution was named as S1. Sodium dodecylbenzene sulfonate (0.10 g) was added into 50 ml deionized water and stirred until it was dissolved completely. The solution was named as S2. S1 and S2 were added into a Teflon-lined autoclave of 200 ml capacity. The mixture was stirred, and then 24 ml of ammonia solution was added as a gelatin agent and stirred. The autoclave was kept at a temperature of 150°C for 12 h. After cooling to room temperature naturally, the products were collected, washed with distilled water and absolute ethanol several times, and dried in a vacuum at 60°C for 4 h. Then, the MH-modified CNTs were obtained and named as MH-CNTs.

2.3 Preparation of MH crystal

Preparation of MH followed the same experimental method as that of MH-CNTs in the absence of CNTs.

2.4 Preparation of control groups

The processing of CNTs followed the same experimental method as that of MH-CNTs in the absence of Mg(NO3)2·6H2 O.

The obtained MH and CNTs were mixed under grinding. The mixture was named as MH+CNTs, which has the same weight ratio as that of MH/CNTs=8:5 (calculated from the reaction ratio) in the MH-CNTs.

2.5 Preparation of EVA composites

All the samples were mixed for 15 min at 150°C in a two-roll mill (SR-160B, Guangdong Zhanjiang Machinery Factory, China). Then, the mixtures were added into a stainless-steel mold at 180°C under a pressure of 10 MPa for 5 min. The formulations of the EVA composites are presented in Table 1.

Table 1

Compositions of the samples.

SamplesEVA (wt%)MH (wt%)CNTs (wt%)MH+CNTs (wt%)MH-CNTs (wt%)
01000000
15050000
25047300
35047030
45047003

2.6 Characterization

A transmission electron microscope (TEM; Tecnai G2 F20, Philips) was used to detect the morphology of MH and MH-CNTs. The samples were prepared by dropping a sample suspension in ethanol on a Cu grid coated with a carbon film. X-ray diffraction (XRD) measurement was performed with a Rigaku DMAX-RC diffractometer (Japan). CuKα radiation (λ=0.15406 nm) was used, and the scanning rate was 2°/min with a generator voltage of 45 kV and a generator current of 180 mA. XRD peaks were recorded from 2θ=5° to 80°. Thermogravimetric analysis (TGA) was carried out using a Rigaku TA-50 instrument (Japan). Samples were heated from room temperature to 700°C at nominal heating rates of 5–20°C/min in an atmosphere of flowing air. The cone calorimeter (Stanton Redcroft, UK) tests were performed according to ISO5660 standard procedures. Each specimen of dimensions 100×100×3 mm3 was wrapped in aluminum foil and exposed horizontally to an external heat flux of 35 kW/m2. The tensile testing of the samples, which were dumbbell-shaped test specimens, was performed at a crosshead speed of 20 mm/min by using a universal testing machine (M350-20KN; Testometric, UK) at room temperature. Five samples were tested for each composite, and the mean value was applied.

3 Results and discussion

XRD measurement was performed to determine the crystalline structure of the particles. Figure 1 illustrates the XRD patterns of (A) MH, (B) CNTs, (C) MH+CNTs, and (D) MH-CNTs.

Figure 1 XRD patterns of (A) MH, (B) CNTs, (C) MH+CNTs, and (D) MH-CNTs.
Figure 1

XRD patterns of (A) MH, (B) CNTs, (C) MH+CNTs, and (D) MH-CNTs.

The diffraction peaks of sample (A) at 2θ=18.5°, 37.9°, 50.8°, 58.6°, 62.1°, and 68.2° correspond to the (001), (101), (102), (110), (111), and (103) reflections of MH crystal, respectively. The diffraction peak of sample (B) at 2θ=26° can be confidently indexed as the (002) reflection of the CNTs. The XRD pattern of sample (C) is a superposition of patterns (A) and (B), as expected. With regard to sample (D), similar peaks with those of MH can be found on the XRD pattern of MH-CNTs, and the diffraction peak of sample (D) at 2θ=26° is the (002) reflection of the CNTs, which is similar with that of sample (B). It is obvious that a lot of weak noise peaks on the patterns of sample (B) and (C) can be found due to the isolated CNTs (or non-modified CNTs). On the contrary, the diffraction peaks of sample (D) are all sharp, and there is not any noise peak. This could be due to the modification of MH on the CNTs surface.

Figure 2 shows the TEM images of (A) MH and (B) MH-CNTs. Flake MH particles with a diameter of nearly 200 nm can be found as shown in Figure 2A, and the MH showed irregular shapes and aggregation. In Figure 2B, the flake MH with a diameter of nearly 10–20 nm on the CNT surface was distributed uniformly and combined closely with the CNTs. Meanwhile, the MH particles were monodispersed on the CNT surface. This also means that the special surface area of MH in the MH-CNTs was enlarged.

Figure 2 TEM images of (A) MH and (B) MH-CNTs.
Figure 2

TEM images of (A) MH and (B) MH-CNTs.

TGA was used to determine the weight ratio of MH and CNTs in MH-CNTs. Figure 3 shows the TGA curves of CNTs, MH, and MH-CNTs. As shown in Figure 3, CNTs had a tiny weight loss of about 5% in the temperature range of 100–800°C, which was attributed to the thermal decomposition of amorphous carbon and residual catalyst in the CNTs. MH started to decompose at about 320°C, and its weight loss was almost 30% at a temperature of 800°C. The onset decomposition temperature of MH-CNTs was a little higher than that of MH. The weight loss of MH-CNTs was 20% approximately in the temperature range of 100–800°C. According to the mechanism of the thermal decomposition of MH, it can be easily obtained that the weight ratio of MH and CNTs in MH-CNTs is around 2:1, which approaches the weight ratio obtained from the reactant ratio.

Figure 3 TGA curves of CNTs, MH, and MH-CNTs.
Figure 3

TGA curves of CNTs, MH, and MH-CNTs.

Figure 4 depicts nonisothermal TGA experiments conducted in air at various heating rates. All the samples underwent two steps of thermal oxidative degradation. The first step involved the dehydration of MH and the loss of acetic acid in EVA at the range of 300–400°C, whereas the second degradation step at a temperature range of 400–550°C was due to the degradation of ethylene-based chains and the volatilization of the residual polymer. The onset temperature (To) is a typical parameter for reflecting the thermal stability of a material. The To of the EVA composites at a heating rate of 10°C/min are given in Table 2. As shown in Table 2, the To of pure EVA was about 351°C, whereas the MH/EVA composite had a To of 358.2°C, which is little larger than that of pure EVA. With the addition of CNTs, the To of CNTs/EVA and MH+CNTs/EVA was 376.6°C and 373.7°C, respectively. MH-CNTs/EVA had the largest To among all the samples, and this suggests a higher thermal stability.

Figure 4 TGA curves of EVA composites under flowing air: (A) pure EVA, (B) MH/EVA, (C) CNTs/EVA, (D) MH+CNTs/EVA, and (E) MH-CNTs/EVA.
Figure 4

TGA curves of EVA composites under flowing air: (A) pure EVA, (B) MH/EVA, (C) CNTs/EVA, (D) MH+CNTs/EVA, and (E) MH-CNTs/EVA.

Table 2

TGA data of the EVA composites.

SamplesTo (°C)E1 (kJ mol-1)E2 (kJ mol-1)
0350.9118.42155.93
1358.2117.35158.98
2376.6118.57163.34
3373.7117.23162.57
4394.1135.59235.46

To investigate the thermal stability more deeply, the kinetics of the thermal degradation of EVA composites were introduced.

The kinetics of the reactions in solid materials are usually described by Eq. (1):

(1)dα/dt=k(T)f(α), (1)

where f(α) is the reaction model, α is the extent of the reaction, k(T) is the Arrhenius rate constant, T is the temperature, and t is the time. For non-isothermal conditions, when temperature varies with time with a constant heating rate, β=dT/dt, Eq. (1) is represented as follows

(2)dα/f(α)=(A/β)exp(-E/RT)dT, (2)

where A is the pre-exponential factor, E is the activation energy, and R is the gas constant. The thermal oxidative aging of cross-linked silicone rubber-based composite is very complicated, and it is difficult to propose a clear mechanism for its oxidative degradation; however, the process can be estimated to a good extent using integral isoconversional methods.

The Flynn-Wall-Ozawa (FWO) method was chosen to obtain the activation energy of the thermal oxidative degradation without knowledge of the particular decomposition mechanism and the reaction order.

The FWO method is an integral method that is based on

(3)logβ=log(AERG(α))-2.315-0.4567ERT, G(α)=∫0αexp(-ERT)dt (3)

Therefore, if series of experiments are carried out at different values of β, the apparent activation energy (E) can be obtained, which is independent of the degradation mechanism. In this case, α=0.05, 0.10, and 0.15 were chosen to evaluate the activation energy of the first thermal oxidative degradation step of EVA composites (E1), and α=0.25, 0.30, 0.35, 0.40, 0.45, and 0.50 were chosen to evaluate the activation energy of the second thermal oxidative degradation step of EVA composites (E2). Equation (3) was used, and the mean values of activation energy obtained from the TGA curves are shown in Table 2.

As shown in Table 2, with regard to pure EVA (sample 0), its E1 was about 118.42 kJ mol-1 and E2 was about 155.93 kJ mol-1. With the addition of MH, the E1 of sample 1 was decreased to 117.35 kJ mol-1, which is smaller than that of pure EVA. This could be due to the decomposition of MH partly instead of EVA in the temperature range of 300–400°C. The E2 of sample 1 was 158.98 kJ mol-1, and larger than that of pure EVA, which is due to the formation of charred residue layers. For sample 2, CNT/EVA composites, the E1 was similar to the E1 of pure EVA, and the E2 was larger than that of pure EVA. These could be due to the high thermal conductivity of CNTs and the formed compact charred layers. The E1 and E2 of the MH+CNTs/EVA sample lied between those of MH/EVA and CNTs/EVA, which was a superposition effect of the two particles. With regard to the MH-CNTs/EVA composite, it had an E1 of 135.59 kJ mol-1, which is much larger that those of the other samples. This increase of E1 could be due to the interaction between MH and CNTs in MH-CNTs. The E2 of the MH-CNTs/EVA composite was about 235.46 kJ mol-1, which is also larger than those of the other samples, and this could be due to the charred layers formed by CNTs.

Tensile strength and elongation at break of EVA composites are shown in Figure 5. The tensile strength of the pure EVA sample was about 17.5 MPa. With the addition of MH, the tensile strength of MH/EVA decreased sharply by around 37% due to the aggregation and poor dispersion of MH. The CNTs/EVA sample (EVA: 50 wt%, MH: 47%, CNTs: 3 wt%) had a tensile strength of about 12.8 MPa, which is higher than that of MH/EVA composite. This could be due to the addition of CNTs. A 3 wt% of the mixture of MH and CNTs (the weight ratio of MH/CNTs was 2:1, which is same as that in MH-CNTs) had a tensile strength of about 12.4 MPa. The tensile strength of the MH+CNTs/EVA sample lay between those of MH/EVA and CNTs/EVA, which was a superposition effect of the two particles. It is obvious that the tensile strength of MH-CNTs/EVA composite is the largest one among all the samples except the pure EVA, and it was about 15.2 MPa. Similar results can be found on the changes of the elongation at break.

Figure 5 Mechanical properties of EVA composites.
Figure 5

Mechanical properties of EVA composites.

A remarkable effect of MH-CNTs on enhancing the mechanical properties of EVA composites can be found. This could be chiefly attributable to two aspects. For one, the presence of CNTs decreased the diameter of the obtained MH on the CNT surface. A smaller and better-dispersed MH improved the mechanical properties of the EVA composites. Meanwhile, owing to the MH, the dispersion of CNTs was also improved, and well-dispersed CNTs could enhance the mechanical properties of the EVA composite. Moreover, the coexistence of MH and CNTs, especially the bond between them, make MH-CNTs more effective than the others. Although MH+CNTs attained a similar ratio with MH-CNTs, the tensile strength of its composite was much lower than that of MH-CNTs.

The cone calorimeter test based on the oxygen consumption principle has been widely used to evaluate the flammability characteristics of materials. The results of the cone calorimeter test correlate well with those obtained from large-scale fire tests and can be used to predict the combustion behavior of materials in real fires. The heat release rate (HRR) measured by the cone calorimeter is a very important parameter as it expresses the intensity of a fire, which in turn determines other parameters. A highly flame-retardant system normally shows a low mean HRR value. The peak of HRR (pk-HRR) value is used to express the intensity of a fire. The dynamic HRR curves of EVA composites versus time are shown in Figure 6.

Figure 6 Dynamic HRR curves of EVA composites.
Figure 6

Dynamic HRR curves of EVA composites.

As shown in Figure 6, pure EVA burns out within 300 s after ignition. A sharp peak can be found on the HRR curve of EVA at the range of 50–250 s, with pk-HRR of about 776 kW/m2. The MH/EVA sample showed a dramatic decline of HRR, and its combustion time was prolonged to around 500 s, and the pk-HRR of the MH/EVA sample was about 498 kW/m2, which is 35.8% lower than that of pure EVA. It can be observed that as a flame retardant, CNTs also decreased the HRR of the EVA composite. The pk-HRR and combustion time of the CNT/EVA composites were around 379 kW/m2 and 800 s, respectively. The combustion time was prolonged sharply. This could be due to the excellent thermal conductivity of CNTs.

The pk-HRR and combustion time of MH+CNTs/EVA composite were about 250 kW/m2 and 800 s, respectively. According to the literature, there is a synergistic effect in the mixture of MH and CNTs on the flame retardancy of EVA. It is obvious that MH-CNTs/EVA had a flat HRR curve, and the pk-HRR was about 150 kW/m2. The HRR almost kept constant from 150 to 700 s, which means that the heat release during the combustion was uniform. MH-CNTs exhibited a more efficient synergistic effect than MH+CNTs on the flame retardancy of EVA.

Future work will aim at investigating the changes of the fillers and matrix during burnings to investigate the synergistic mechanism of MH-CNTs on flame retardant EVA.

4 Conclusion

Considering all the above analysis, it can be concluded that (i) the presence of CNTs affected the size of attaching MH, which was changed from about 200 to 20 nm. MH also had an enlarged special surface area in the MH-CNTs; (2) the synergistic effect was found in the MH-CNTs on the flame retardant EVA, and made MH-CNTs a more effective fire retardant additive than the others. The TGA data showed that MH-CNTs/EVA had the highest thermal stability among the other samples, and the activation energy of the thermal oxidative degradation of MH-CNTs/EVA (obtained through the FWO method) also indicated improved thermal oxidative stability. The tensile strength of the EVA filled with MH-CNTs decreased by only 16%. The results from the cone calorimeter test showed that the heat release during the burning of MH-CNTs/EVA was sharply decreased, and the flame retardancy properties were improved.

Corresponding author: Hongyan Li, School of Materials Science and Engineering, Tianjin Chengjian University, Tianjin 300384, P.R. China, e-mail:

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Received: 2014-5-5
Accepted: 2014-5-25
Published Online: 2014-8-27
Published in Print: 2016-1-1

©2016 by De Gruyter

Articles in the same Issue

  1. Frontmatter
  2. Review
  3. The behaviour of aluminium matrix composites under thermal stresses
  4. Original articles
  5. Preparation and characterization of graphite/resin composite bipolar plates for polymer electrolyte membrane fuel cells
  6. Synergistic effect of carbon nanotubes in combination with magnesium hydroxide on the flame retardant poly(ethylene-co-vinyl acetate)
  7. Preparation and characterization of nano biphasic calcium phosphate/poly-L-lactide composite scaffold
  8. Durability study of ramie fiber fabric reinforced phenolic plates under humidity conditions
  9. Synthesis and molecular dynamics simulation of hyperbranched poly(amine-ester)/neodymium nanocomposites
  10. Investigation on wear properties of AZ31-MWCNT nanocomposites fabricated through mechanical alloying and powder metallurgy
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  12. Analysis of shrinkage and creep behaviors in polymer-coated lightweight concretes
  13. Investigation of optimum cutting parameters and tool radius in turning glass-fiber-reinforced composite material
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  15. Free vibration and postbuckling of laminated composite Timoshenko beams
https://doi.org/10.1515/secm-2014-0135
Keywords for this article
carbon nanotubes; flame retardancy; magnesium hydroxide; poly(ethylene-co-vinyl acetate); synergistic effect

Articles in the same Issue

  1. Frontmatter
  2. Review
  3. The behaviour of aluminium matrix composites under thermal stresses
  4. Original articles
  5. Preparation and characterization of graphite/resin composite bipolar plates for polymer electrolyte membrane fuel cells
  6. Synergistic effect of carbon nanotubes in combination with magnesium hydroxide on the flame retardant poly(ethylene-co-vinyl acetate)
  7. Preparation and characterization of nano biphasic calcium phosphate/poly-L-lactide composite scaffold
  8. Durability study of ramie fiber fabric reinforced phenolic plates under humidity conditions
  9. Synthesis and molecular dynamics simulation of hyperbranched poly(amine-ester)/neodymium nanocomposites
  10. Investigation on wear properties of AZ31-MWCNT nanocomposites fabricated through mechanical alloying and powder metallurgy
  11. Probabilistic analysis of a thermosetting pultrusion process
  12. Analysis of shrinkage and creep behaviors in polymer-coated lightweight concretes
  13. Investigation of optimum cutting parameters and tool radius in turning glass-fiber-reinforced composite material
  14. Buckling and vibration analyses of composite laminates with weak interfaces by a coupled meshfree and finite element method
  15. Free vibration and postbuckling of laminated composite Timoshenko beams
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