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Significantly improving the performance and dispersion morphology of porous g-C3N4/PANI composites by an interfacial polymerization method

  • Qingbo Yu , Xianhua Li EMAIL logo , Leigang Zhang , Xuexue Wang , Yulun Tao and Mingxu Zhang
Published/Copyright: February 10, 2015
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e-Polymers
From the journal e-Polymers Volume 15 Issue 2

Abstract

Polyaniline (PANI) nanorods grown on layered porous graphitic carbon nitride (porous g-C3N4) sheets (porous g-C3N4/PANI) were successfully synthesized by interfacial polymerization of aniline monomers in the presence of porous g-C3N4 sheets. The experimental results suggest that porous g-C3N4 obtained a good dispersion with intercalated and exfoliated nanostructure and interfacial adhesion in PANI, which improved the thermal stability and photocatalytic activity of the porous g-C3N4/PANI composites.

Keywords: dispersion; interfacial polymerization; photocatalytic performance; porous g-C3N4/PANI composites; thermal stability

1 Introduction

Graphitic carbon nitride (g-C3N4) has attracted considerable attention as a visible light photocatalyst because of its narrow band gap of 2.7 eV, plentiful material source, superior physicochemical and photochemical stabilities, and cost-effectiveness in synthesis (1). Compared with other organic π-conjugated materials, g-C3N4 is crystalline owing to its lamellar structure, which promotes charge transfer. Yet the obtained visible light photocatalytic activity of pure g-C3N4 is very low because of the contact resistance between the sheets and the marginal visible light absorption (2–4). Extensive efforts have been directed toward enhancing the photocatalytic activity of g-C3N4, such as compositing g-C3N4 with HCl (5) and other semiconductors (6), and constructing heterojunctions (7). Zhang et al. (8–11) composed g-C3N4 with a semiconductor material (Ag-AgCl, ZnFe2O4) doped with nonmetal and metal ion. They conclude that high-performance photocatalysts can be obtained by fast separation of photogenerated electron-hole pairs (8–11). Ge et al. (12–14) reported cobalt-phosphate-modified g-C3N4 photocatalysts, Co3O4-g-C3N4 heterojunction photocatalysts, and molybdenum disulfide/g-C3N4 composites. They also found that the efficient separation of electron-hole pairs can promote the photocatalytic activity of g-C3N4 (12–14).

Polyaniline (PANI) has received increasing attention in photocatalysis and solar energy conversion because of its high absorption coefficient and charge carriers in the visible-light range (15). PANI and g-C3N4 have a π-conjugated structure, which makes them the most compatible materials to form composites. Most importantly, the resultant composites have an improved photocatalytic activity. Ge et al. (16) reported a PANI-modified g-C3N4 composite synthesized by an in situ method that expounded a visible light photocatalytic activity toward the degradation of methylene blue (MB). Zhang et al. recently used the same method to fabricate hierarchical nanocomposites, resulting in an enhanced optoelectronic conversion performance (15). However, their work offers no information regarding the thermal stability of composites after PANI with weaker thermal stability is introduced, which is significant in commercial applications. In addition, in their research, accumulation tends to form. Importantly, both PANI and g-C3N4 are insoluble. So, well-distributed g-C3N4/PANI composites cannot be acquired via conventional process methods.

In this work, we report an interfacial polymerization method to fabricate PANI nanorods grown on porous graphitic carbon nitride sheets with good dispersion. The composites were characterized by Fourier transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy, X-ray diffraction (XRD), UV-Vis, thermogravimetry analysis (TGA), and electrochemical measurements, respectively. The resulting composites exhibited not only improved thermal stability, but also enhanced photocatalytic performance. Furthermore, related mechanisms are also discussed.

2 Experimental part

2.1 Materials

All of the reagents were of analytical grade (Tianjin Kermel Chemical Reagents Development Centre, Tianjin, China) and were used without further purification. Porous g-C3N4 was prepared based on literature procedures (17). ITO glass was purchased from Geao Co. (Shanghai, China).

2.2 Preparation of porous g-C3N4/PANI

The composites were synthesized by interfacial polymerization in the presence of aniline monomer and porous g-C3N4 sheets. A typical procedure was as follows: 3 mg of porous g-C3N4 sheets was added into 20 ml of HCl solution (0.5 mol/l). At the same time, 1.4 mmol of aniline monomers was dissolved in carbon tetrachloride (10 ml). Then, the two compounds were mixed and sonicated to obtain good dispersion (3 h). Then 0.285 g of ammonium persulfate (APS) was slowly added to the above mixture and then cooled to 0°C. The reaction was executed at the interface of the two phases at 0° for 24 h. The mixture was precipitated by acetone. The precipitates were filtered and washed with deionized water and ethanol, respectively, and finally dried under vacuum. For comparison, PANI nanorods were fabricated via a similar procedure without the presence of porous g-C3N4 sheets.

2.3 Photocatalytic experiment

The photocatalytic activity of the various photocatalysts (5 mg) was measured by monitoring the degradation of an aqueous suspension of MB (50 ml, 10 mg/l) in a beaker. The light irradiation system consisted of a 300-W Xe lamp with a cut-off filter for visible light (λ>400 nm). A radiometer (FZ-A, Photoelectric Instrument Factory Beijing Normal University) was used to measure the visible light intensity. The intensity was 100 μW/cm2. Before the irradiation, the photocatalysts were blended with the MB under dark conditions. The MB concentrations were monitored, as shown in Figure S1. The MB remained unchanged after 20 min. So, the photocatalysts were blended with the MB under dark conditions for 20 min in the subsequent experiment. At the predetermined irradiation time, 3 ml of the samples was collected. The MB concentrations were measured using a UV-Vis spectrophotometer.

2.4 Characterization

SEM images were obtained using an S4800 scanning electron microscope (Hitachi Co., Japan). TGA of the samples was performed on a Q2000 thermogravimetric analyzer (Mettler-Toledo International Inc., Switzerland) at a heating rate of 10°C/min in argon gas. FTIR (Bruker Company, Germany) and XRD (Bruker Company, Germany) were used to obtain structural information about the samples and performed using a NEXUS-870 spectrophotometer and a Rigaku RINT2000 diffractometer, respectively. UV-Vis diffuse reflection spectra were obtained with a UV-Vis spectrophotometer (Varian CARY100, USA). The electrochemical measurements were performed on a CHI 660E (CH Instruments, Inc., Shanghai, China) electrochemical workstation by using three-electrode cells.

3 Results and discussion

The PANI loaded on the porous g-C3N4 sheet can be confirmed by X-ray diffraction (Figure 1A). The neat PANI shows partial crystallinity with at least three Bragg diffraction peaks (curve 2 in Figure 1A); the crystalline reflex at 2θ=15° is indicative of the crystalline structure of the emeraldine salt 1 (ES1) type (18). The broad bands centered at 2θ=20.42° and 25.38° are the characteristic Bragg diffraction peaks of PANI (15). For porous g-C3N4 (curve 1 in Figure 1A), the XRD peak at 27.5 can be indexed as the (002) diffraction plane, which belongs to the stacking distance of the conjugated aromatic system. Another pronounced additional peak was found at 13.1, relating to an in-plane structural packing motif, such as the hole-to-hole distance of the nitride pores in the crystal. In the case of porous g-C3N4/PANI composite (curve 3 in Figure 1A), the peak of the porous g-C3N4 sheet stacking disappeared, suggesting that the porous g-C3N4 has almost no aggregation and is fully used as the substrate of PANI to produce composites. Two broad peaks of the porous g-C3N4/PANI composite centered at 2θ=20.12° and 25.26° were almost the same as that of pure PANI.

Figure 1 (A) XRD and (B) FTIR spectra of porous g-C3N4 (1):PANI (2), and porous g-C3N4/PANI composite (3).
Figure 1

(A) XRD and (B) FTIR spectra of porous g-C3N4 (1):PANI (2), and porous g-C3N4/PANI composite (3).

The composite structure was further proved by spectroscopy measurement. Figure 1B shows the FT-IR spectra of the samples. The IR absorption bands in the porous g-C3N4 sample revealed a typical molecular structure of g-C3N4 (curve 1 in Figure 1B). The numerous intense bands in the 1249–1630 cm-1 regions corresponded to the typical stretching modes of the CN heterocycles. The intense band at 807 cm-1 represented the characteristic breathing modes of the triazine units (17). Compared with porous g-C3N4, two new peaks appeared in the spectrum of the porous g-C3N4/PANI composite (curve 3 in Figure 1B). The one at 1459 cm-1 was almost the same as that of pure PANI (curve 2 in Figure 1B), which was attributed to the vibration of C=C. The other peak at 1139 cm-1, which shifted toward a longer wavelength compared with PANI, was attributed to the vibration of C-H (16). Meanwhile, the characteristic breathing modes of the triazine units at 807 cm-1 were strengthened after PANI was introduced. The results indicate that an interaction was formed between PANI and porous g-C3N4.

The morphology of porous g-C3N4, PANI, and porous g-C3N4/PANI samples was investigated by SEM. In Figure 2A, the porous g-C3N4 shows a typical porous morphology in each sheet. For PANI (Figure 2B), random stacking clubbed morphology with a diameter in the range of 40–60 nm was obtained. When PANI was coupled with porous g-C3N4 (Figure 2C), PANI nanorods were arrayed on the porous g-C3N4 nanosheet. No porous g-C3N4 nanosheet was obtained from the composite structures, and porous g-C3N4 facets closely coupled with PANI nanorods were observed, suggesting a powerful interfacial bonding between porous g-C3N4 and PANI (19). This result is consistent with those of XRD and FT-IR characterizations.

Figure 2 Typical SEM images of porous g-C3N4 (A), PANI (B), and porous g-C3N4/PANI composite (C).
Figure 2

Typical SEM images of porous g-C3N4 (A), PANI (B), and porous g-C3N4/PANI composite (C).

A formation mechanism of porous g-C3N4/PANI composites is illustrated in Scheme 1. At first, the oxidant (APS) and porous g-C3N4 exist in the aqueous phase and aniline monomers are dissolved in the organic phase. Then polymerization of aniline happens and aniline oligomers are formed at the interface, and the oligomers diffuse to the aqueous phase. The π-π electron stacking interaction between the aniline oligomers and the basal planes of porous g-C3N4 leads to PANI to assemble onto the surface of the porous g-C3N4 (20, 21). When aniline oligomers further develop, intermolecular interaction becomes strong. Facet coupling of PANI nanorod arrays on graphitic carbon nitride sheets is obtained.

Scheme 1 Schematic presentation of the fabrication of porous g-C3N4/PANI composite.
Scheme 1

Schematic presentation of the fabrication of porous g-C3N4/PANI composite.

The TGA curves of porous g-C3N4, PANI, and porous g-C3N4/PANI composite under Ar atmosphere are plotted in Figure 3A. For PANI (curve 1 in Figure 3A), the first mass loss stage below 100°C belongs to the evaporation of the physically adsorbed H2O molecules. Afzal et al. (22) also reported a similar trend for PANI/Au nanocomposites. The weight loss from 100°C to 400°C was ascribed to the removal of water and dopant molecules adsorbed on PANI and to the degradation of the oligomers. The main weight loss happened after 400°C, suggesting the decomposition of the molecular chains of the polymer. In Ar atmosphere, porous g-C3N4 followed a single-step degradation process (curve 3 in Figure 3A). It is obvious that porous g-C3N4/PANI composites (curve 2 in Figure 3A) not only became more resistant to thermal degradation in comparison to PANI, but also had much lower char residue at 883°C than porous g-C3N4 and PANI. Several literature studies have shown that materials with high aspect ratio and surface area in composites offered a tortuous path for the diffusion of gas and, more importantly, reduced the permeation rate of gas (23). So, the porous g-C3N4 sheets with exfoliated and intercalated nanostructure in composites, caused by the interfacial polymerization method, acted as a physical barrier and delayed the escape of the degradation products (24). The conjugate interactions can also increase the thermal degradation activation energy of porous g-C3N4/PANI composites by restricting the thermal motion of the polymer chains (25). Another factor is the higher thermal stability of porous g-C3N4. Thus, the composites possess better thermal stability.

Figure 3 (A) TGA curves and (B) UV-Vis absorption spectrum of PANI nanorods (1), porous g-C3N4/PANI composite (2), and porous g-C3N4 (3).
Figure 3

(A) TGA curves and (B) UV-Vis absorption spectrum of PANI nanorods (1), porous g-C3N4/PANI composite (2), and porous g-C3N4 (3).

The optical absorption of porous g-C3N4, PANI, and porous g-C3N4/PANI composites was studied by UV-Vis absorption spectroscopy (Figure 3B). Compared with porous g-C3N4 (curve 3 in Figure 3B), porous g-C3N4/PANI composites (curve 2 in Figure 3B) increased their light absorption over the entire range of wavelengths investigated, which is a typical behavior of PANI (15). Therefore, we can deduce that the introduction of PANI was able to absorb more light, exhibiting improved catalytic activity.

The transient photocurrents of porous g-C3N4 and porous g-C3N4/PANI composites were surveyed during recurrent on/off illumination cycles. The samples show expeditious and reproducible photocurrent responses on every illumination (Figure 4A). When the irradiation was cut off, the photocurrent quickly dropped to almost zero (steady-state value) but returned to the original value as soon as the light was switched back on. The transient photocurrent density of the porous g-C3N4/PANI composites was more than 4.3 μA/cm2 (curve 1 in Figure 4A), yet that of the porous g-C3N4 was <1.2 μA/cm2 (curve 2 in Figure 4A). The photocurrent density of the porous g-C3N4/PANI composites was about 3.58 times higher than that of the porous g-C3N4 composite. This result suggests the significant effect of PANI in improving electron shuttling and in restraining charge recombination, where PANI acts as an electron transfer channel, transferring the photogenerated electrons from g-C3N4 (16).

Figure 4 Photocurrent densities (A) and electrochemical impedance spectroscopy changes (B) of porous g-C3N4/PANI composite (1) and porous g-C3N4 (2).
Figure 4

Photocurrent densities (A) and electrochemical impedance spectroscopy changes (B) of porous g-C3N4/PANI composite (1) and porous g-C3N4 (2).

In order to obtain a further insight into the charge transport behavior of porous g-C3N4 and porous g-C3N4/PANI composites, we performed electrochemical impedance spectroscopy measurements (Figure 4B). In the Nyquist diagram, the radius of every arc is connected to the charge-transfer process and a bigger radius corresponds to a higher charge-transfer resistance (26). Porous g-C3N4/PANI composites exhibited smaller charge-transfer resistance with the introduction of PANI, indicating a faster charge transfer between g-C3N4 and PANI.

The photocatalytic activities of porous g-C3N4 and porous g-C3N4/PANI composites were evaluated by MB photodegradation under visible light (>400 nm) irradiation. From Figure 5A, without any catalyst, the MB decomposition rate was about 5% after 180 min of illumination, which can be accounted for by the natural photodegradation of the MB molecules. For the porous g-C3N4 photocatalyst, about 30% MB was degraded after 120 min of illumination, while 70% MB was degraded using porous g-C3N4/PANI as the photocatalyst. The enhancement of photocatalytic performance can be attributed to the improved visible light utilization, oxidation power, and electron transport property, due to the synergistic effect of facets coupling PANI and g-C3N4.

Figure 5 (A) Process of photocatalytic degradation of MB under visible light irradiation (λ>400 nm); (B) first-order plots for the photodegradation of MB; (C) recycle test of the porous g-C3N4/PANI composite catalyst.
Figure 5

(A) Process of photocatalytic degradation of MB under visible light irradiation (λ>400 nm); (B) first-order plots for the photodegradation of MB; (C) recycle test of the porous g-C3N4/PANI composite catalyst.

To quantitatively investigate the reaction kinetics of the MB degradation, the experimental data were further fitted by applying a first-order model. As shown in Figure 5B, the plot of the irradiation time (t) against ln(C0/Ct) is nearly a straight line in both samples. The reaction constant k of the porous g-C3N4/PANI composites, which was used to evaluate the degradation rate, was almost 3.3 times that of porous g-C3N4 under visible light irradiation, suggesting that the enhanced photocatalytic activity contributed to the efficient light absorption.

Figure 5C shows that the photocatalytic activity of the porous g-C3N4/PANI composites is stable for each cycle under the same conditions, although a small decline (2%) can be detected after three cycles.

4 Conclusions

In summary, an interfacial polymerization method that synthesizes porous g-C3N4/PANI composites was developed, which allows porous g-C3N4 to achieve good dispersion with exfoliated and intercalated nanostructure and interfacial adhesion in PANI. This significant structure not only improves the thermal stability of the composites, but also enhances the photocatalytic activity toward the photocatalytic degradation of MB.

Corresponding author: Xianhua Li, School of Mechanical Engineering, Anhui University of Science and Technology, Huainan 232001, P.R. China, Fax: +86-0554-6313991, e-mail: ; and Department of Materials Science and Engineering, Anhui University of Science and Technology, Huainan 232001, P.R. China

Acknowledgments

This work was supported by the National Nature Science Foundation of China (21401001) and the Anhui Province Key Laboratory of Environment-Friendly Polymer Materials.

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Supplemental Material

The online version of this article (DOI: 10.1515/epoly-2014-0218) offers supplementary material, available to authorized users.

Received: 2014-12-3
Accepted: 2015-1-2
Published Online: 2015-2-10
Published in Print: 2015-3-1

©2015 by De Gruyter

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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https://doi.org/10.1515/epoly-2014-0218
Keywords for this article
dispersion; interfacial polymerization; photocatalytic performance; porous g-C3N4/PANI composites; thermal stability
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Articles in the same Issue

  1. Frontmatter
  2. In this Issue
  3. Editorial
  4. Editorial March 2015
  5. Full length articles
  6. Biodegradable silk fibroin/chitosan blend microparticles prepared by emulsification-diffusion method
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