Preparation and Catalytic Activity of M<sub>2</sub>O<sub>3</sub>/CNTs (M = Y, Nd, Sm) Nanocomposites by Solvothermal Process

Zhang, Xiaojuan; Hao, Lingyun

doi:https://doi.org/10.1155/2018/3635164

Journal of Nanomaterials

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Abstract Introduction Experimental Results and Discussion Conclusions Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

Research Article | Open Access

Volume 2018 | Article ID 3635164 | https://doi.org/10.1155/2018/3635164

Preparation and Catalytic Activity of M₂O₃/CNTs (M = Y, Nd, Sm) Nanocomposites by Solvothermal Process

Xiaojuan Zhang^1,2and Lingyun Hao^1,2

Academic Editor: Andrew R. Barron

Received04 Jan 2018

Revised09 Mar 2018

Accepted04 Apr 2018

Published11 Jun 2018

Abstract

The rare-earth oxide nanoparticles along carbon nanotubes (CNTs) (M₂O₃/CNTs, M = Y, Nd, Sm) were prepared by in situ solvothermal method. Products were characterized by infrared spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray spectrometry, scanning electron microscopy, and Brunauer-Emmett-Teller method. M₂O₃/CNTs presented good morphology and large surface area. Furthermore, catalysis of M₂O₃/CNTs during the thermal decomposition of ammonium perchlorate (AP) was evaluated by differential thermal analysis (DTA). Compared with Nd₂O₃/CNTs and Sm₂O₃/CNTs, Y₂O₃/CNTs nanocomposites showed the best catalytic effect on the thermal decomposition of AP. With the addition of 2 wt.% Y₂O₃/CNTs nanocomposite, high decomposition temperature of AP decreased by 125.5°C, and the total DTA heat release increased by 2.027 kJ·g⁻¹.

1. Introduction

Rare-earth oxide (M₂O₃) nanoparticles have received considerable attention because of their applications in various fields, such as advanced ceramics, superconducting materials, luminescence materials, oxygen sensor, and catalysis [1–4]. In the past years, all kinds of one-dimensional and two-dimensional rare-earth nanostructures, such as rods, wires, tubes, and plates, have been synthesized by numerous groups [5, 6]. M₂O₃ nanoparticles exhibit good catalytic effect in the thermal decomposition of ammonium perchlorate (AP) [7], which is used as oxidizer in solid propellants [8–10]. However, M₂O₃ nanoparticles exhibit agglomeration, which negatively influences their catalytic properties in propellants.

Owing to their unique electronic and physical properties [11, 12], carbon nanotubes (CNTs) may act as a catalyst support, on which nanoparticles may be attached to improve catalytic effect [13, 14]. M₂O₃/CNT nanocomposites have been prepared through numerous methods, such as chemical deposition, sol-gel, hydrothermal, atmospheric-pressure-plasma jet, and electrophoretic deposition [15–17]. For example, Wu and Chen prepared plasma-resistant Y₂O₃/CNT nanocomposites by an atmospheric-pressure-plasma jet method [18]. Y₂O₃/CNTs composites with high conductivity can be prepared in 3–5 s using atmospheric-pressure-plasma jet method, and the conventional furnace calcination would take 10–15 min at 400–500°C. And CNTs-doping has been found to be an effective method to improve the conductivity of Y₂O₃. Zhao et al. synthesized Nd₂O₃/CNT nanocomposites through chemical deposition and calcination [19]. With the surfactant served as a “bridge” between Nd(OH)₃ and CNTs, the Nd₂O₃ nanoparticles with average particle size of 30–40 nm can be deposited on the surface of CNTs. And the obtained Nd₂O₃/CNTs had higher specific area and exhibited better catalysis on the thermal decomposition of AP. Mo et al. synthesized Eu₂O₃/CNT structures via electrophoretic deposition [20]. The electrophoretic deposition techniques produced densely packed CNTs mat-Eu₂O₃ film-CNTs mat heterostructure, and the capacitance-voltage measurements of the CNT mat-Eu₂O₃ film-CNT mat structure confirmed electrical insulation between the two CNT mats and the charge-storage capabilities of the structure.

However, some of these methods lack good control of the morphology of M₂O₃ nanoparticles, whereas others require complex processes, expensive experimental device, or long time. Among the different methods, the solvothermal method [21] is highly advantageous because of its convenient processing, simple experimental equipment, no calcination requirement, and good dispersibility in products.

However, reports on preparing M₂O₃/CNTs by in situ solvothermal method to catalyze the thermal decomposition of AP are limited. In this thesis, we coated M₂O₃ (M = Y, Nd, Sm) nanoparticles on the surface of functional CNTs and studied their catalytic properties by differential thermal analysis (DTA).

2. Experimental

2.1. Materials

Pristine CNTs (diameter: 40–60 nm, purity: 95–98%) were purchased by Shenzhen Nanotechnologies Co., Ltd. Hexadecyl trimethyl ammonium bromide (CTAB), poly(sodium 4-styrenesulfonate) (PSS), yttrium nitrate (Y(NO₃)₃·6H₂O), neodymium nitrate (Nd(NO₃)₃·nH₂O), samarium nitrate (Sm(NO₃)₃·6H₂O), ethylene glycol (EG), NaAc, and polyethylene glycol were of analytical grade and obtained from Shanghai Chemical Company.

2.2. Synthesis of M₂O₃/CNTs Nanocomposites (M = Y, Nd, Sm)

The synthesis of M₂O₃/CNTs nanocomposites is shown in Figure 1. Pristine CNTs were purified in HNO₃ at 140°C for 4 h. Afterwards, the solution was diluted with distilled water and rinsed for several times until the pH value reaches neutral. Then the purified CNTs were modified via polymer wrapping technique, where cationic CTAB (1 g) was adsorbed on CNTs to create a charged template, and anionic PSS (0.24 g) was subsequently grafted onto the surfaces of CNTs. The mixture of CNTs modified by CTAB and PSS was obtained and called functionalized CNTs (f-CNTs).

Around 0.03 g of f-CNTs and 0.2 g of M(NO₃)₃·6H₂O (M = Y, Nd, Sm) were dissolved in 50 mL ethylene glycol (EG). Then, 3.6 g of NaAc and 1 g of polyethylene glycol ( = 4000 g·mol⁻¹) were added with stirring for 0.5 h. The reaction system was heated to 200°C for 2.5 h in an oil bath. Finally, the M₂O₃/CNT (M = Y, Nd, Sm) nanocomposites were press-filtered, washed with ethanol, and dried at 40°C. The respective ratios of M₂O₃ : f-CNTs in experiment were labeled in Table 1.

For comparison, M₂O₃/CNTs nanocomposites were prepared by chemical deposition. f-CNTs and M(NO₃)₃·6H₂O (M = Y, Nd, Sm) were dispersed in 50 mL of distilled water, and sodium hydroxide (NaOH) was dropped into the solution and reacted at 40°C for 1 h. Finally, the product was washed, dried, and calcined in a muffle furnace at 800°C for 2 h.

2.3. Catalytic Activity Measurement

For investigating the catalytic effect of M₂O₃/CNTs nanocomposites, the mass content of M₂O₃/CNTs nanocomposites added in AP was 2 wt.%, and the catalytic performance of f-CNTs was also carried out in the same way as comparison.

2.4. Characterization

The structure was characterized by X-ray diffraction (XRD, Bruker D8). A Bruker VECTOR 22 spectrometer was used to measure infrared (IR) spectrum. The morphology and EDS were measured by scanning electron microscopy (SEM, Model S-8010) and transmission electron microscopy (TEM, Tecnai 12). A Beckman Coulter SA3100 was used to measure the Brunauer-Emmett-Teller (BET) surface areas, and DTA was characterized by a thermal analyzer (TA2100, America).

3. Results and Discussion

3.1. Materials Characterization

3.1.1. IR Analysis

The IR spectra of (a) pristine CNTs and (b) f-CNTs are shown in Figure 2. In Figure 2(a), stretching vibration of O-H appeared at 3480 cm⁻¹. In Figure 2(b), characteristic absorption bands of O-H stretching vibration appeared at 3285 cm⁻¹, and the peaks at 1714 cm⁻¹ can be ascribed to the stretching vibration of C=O bond [22]. In addition, the peaks at 1563 and 1194 cm⁻¹ can correspond to stretching vibration peak of and C-O characteristic bands, respectively. Therefore, f-CNTs were successfully modified by HNO₃.

3.1.2. XRD Analysis

Figure 3 illustrates the XRD patterns of f-CNTs and M₂O₃/CNT nanocomposites. In Figure 3(d), the peaks at 2θ = 22.94° correspond to the (002) plane of f-CNTs (JCPDS No. 25-0284) [18]. From Figures 3(a) and 3(c), characteristic peaks of CNTs remain. In Figure 3(a), diffraction peaks at 29.4°, 33.9°, 40.9°, 48.7°, and 57.9° correspond to the (222), (400), (322), (440), and (622) planes of Y₂O₃ (JCPDS No. 74-1828), respectively [18]. In Figure 3(b), reflection peaks at 26.9°, 29.7°, 30.7°, 40.5°, 47.4°, 53.4°, and 53.4° can be indexed to the (100), (002), (101), (102), (110), (103), and (112) planes of hexagonal Nd₂O₃ (JCPDS No. 41-1089), respectively [19]. As shown in Figure 3(c), reflection peaks appearing at 28.2°, 32.7°, 38.6°, 45.4°, and 54.3° correspond to (222), (400), (332), (521), and (541) planes of cubic Sm₂O₃ (JCPDS No. 15-0813), respectively. As shown in Table 1, the crystallite size of Y₂O₃ deposited on CNTs calculated according to the Scherrer formula is 42 nm and those of Nd₂O₃ and Sm₂O₃ are 34 nm and 20 nm. The crystallite size of Y₂O₃ deposited on CNTs is bigger than that of Nd₂O₃ and Sm₂O₃, which is consistent with the broad peaks in case of Nd₂O₃/CNTs and Sm₂O₃/CNTs.

3.1.3. SEM Analysis

Morphology was investigated by SEM. Figure 4(a) reveals f-CNTs with a diameter of 40–60 nm and good dispersibility. In Figure 4(b), f-CNTs were decorated with a dense layer of Y₂O₃ nanoparticles. Figure 4(c) shows that Nd₂O₃ nanoparticles were homogeneously distributed over f-CNTs because the modified CNTs are covered with a negatively charged surfactant, which can ensure good coverage of positively charged Nd³⁺ by electrostatic attraction. In addition, Sm₂O₃ nanoparticles were loaded on f-CNTs, indicating a strong interaction between Sm₂O₃ nanoparticles and CNTs by surfactant modification (Figure 4(d)). The formation of M₂O₃/CNTs nanocomposites can be represented as follows:M³⁺ in the solution can favorably bind with f-CNTs by electrostatic attraction, and M³⁺ was hydrolyzed to M(OH)₃. As a result, M₂O₃ nanoparticles were anchored onto the surface of f-CNTs. It could be included that the modification of CNTs improved the heterogeneous nucleation; the enhanced nucleation rate favored the generation of much more nuclei and the formation of smaller M₂O₃ nanoparticles.

(a)

(b)

(c)

(d)

3.1.4. EDS Analysis

Energy-dispersive X-ray spectrometry (EDS) was used to measure the composition of M₂O₃/CNT nanocomposites. The peaks (2.2 keV and 2.9 keV) are originated from Au/Pd coating. Figure 5(a) shows that Y₂O₃/CNTs includes 21.75 wt.% of Y, 25.33 wt.% of O, and 52.92 wt.% of C. In Figure 5(b), Nd₂O₃/CNTs contains 13.10 wt.% of Nd, 31.82 wt.% of O, and 55.08 wt.% of C. As shown in Figure 5(c), Sm₂O₃/CNTs contained 11.60 wt.% of Sm, 24.53 wt.% of O, and 63.87 wt.% of C.

(a)

(b)

(c)

According to the results, the relative proportions of f-CNTs and M₂O₃ during the final products by solvothermal process and chemical deposition were listed in Table 1. As shown in Table 1, the relative proportions of M₂O₃ and f-CNTs by chemical deposition were smaller than that of solvothermal process, which indicated that the M₂O₃ nanoparticles had better coverage on f-CNTs by solvothermal process.

3.1.5. TEM Analysis

The morphology of M₂O₃/CNT nanocomposites was further measured by TEM as shown in Figure 6. Figure 6(a) shows TEM image of f-CNTs. Before the reaction, f-CNTs present well-graphitized walls. In Figure 6(b), Y₂O₃ nanoparticles attached to f-CNTs reveal slight nonuniformity and no free nanoparticles. The average particle size of Y₂O₃ nanoparticles was 30 nm, which is considerably smaller than that of Y₂O₃/CNTs produced by chemical deposition (70 nm). In Figure 6(c), Nd₂O₃ nanoparticles supported on f-CNTs exhibited good dispersibility and sphericity. The average particle size of Nd₂O₃ nanoparticles was 45 nm, which was markedly smaller than that of Nd₂O₃/CNTs (90 nm) produced by chemical deposition. In addition, although the coverage of Sm₂O₃ nanoparticles onto f-CNTs is nonuniform, no free nanoparticles were found. And the average particle size of Sm₂O₃ nanoparticles was 90 nm, which is smaller than that of Sm₂O₃/CNTs (120 nm) produced by chemical deposition. The smaller particle size of M₂O₃/CNTs prepared by in situ solvothermal process is advantageous in catalysis.

(a)

(b)

(c)

(d)

3.1.6. BET Analysis

The surface area of M₂O₃/CNT nanocomposites was also characterized. As shown in Table 1, the BET surface area of Y₂O₃/CNTs prepared by solvothermal process was 84 m²·g⁻¹, which is considerably larger than that of Y₂O₃/CNTs produced by chemical deposition (74 m²·g⁻¹) and f-CNTs (33 m²·g⁻¹). The same finding was confirmed by measuring the surface area of Nd₂O₃/CNTs and Sm₂O₃/CNTs nanocomposites. The BET surface areas of Nd₂O₃/CNTs and Sm₂O₃/CNTs were 77 and 65 m²·g⁻¹, which were markedly larger than those of Nd₂O₃/CNTs (41 m²·g⁻¹) and Sm₂O₃/CNTs (58 m²·g⁻¹) produced by chemical deposition. The large BET surface area of M₂O₃/CNTs is advantageous in catalysis.

3.2. Catalytic Properties

3.2.1. DTA Analysis

In Figure 7(a), the transition from orthorhombic to cubic AP is in agreement with the endothermic peak at 245.2°C [23]. The thermal decomposition of AP to form volatile products corresponds to the exothermic peaks at 331°C and 452°C [24]. In Figure 7(b), the two exothermic peaks combine into one peak, and the high thermal decomposition temperature decreases substantially. With the addition of f-CNTs, the high decomposition temperature decreased by 97.4°C, and the total DTA heat release increased by 0.346 kJ·g⁻¹. Compared with f-CNTs, M₂O₃/CNTs nanocomposites showed better catalytic activity (Figures 7(c) and 7(d)). Based on this result, we can deduce that f-CNTs can mainly accelerate the high decomposition of AP, because the violent decomposition of temperature was greatly reduced during this process.

It has been reported that many nanomaterials could catalyze the thermal decomposition of AP. For example, Fe₃O₄ and Co₃O₄ microspheres were synthesized by the hydrothermal reaction and with the addition of 2% Fe₃O₄ and Co₃O₄ microspheres could decrease the high thermal decomposition temperature of AP by 80°C and 55°C, respectively [25]. V₆O₁₃ nanobelts were controlled and synthesized by one-pot hydrothermal process and the high decomposition temperature of AP in the presence of 3% V₆O₁₃ was reduced by 67°C [26]. Zhang et al. improved the catalytic activity of α-Fe₂O₃ in the decomposition of AP by coating amorphous carbon on α-Fe₂O₃ surface, which reduced the high decomposition temperature of AP by 109°C [27].

As shown in Figures 7(c), 7(d), and 7(e), addition of 2.0 wt.% of Y₂O₃/CNTs, Sm₂O₃/CNTs, and Nd₂O₃/CNTs decreased the high thermal decomposition temperature of AP by 125.5°C, 118.4°C, and 123.8°C, respectively, and increased the total DTA heat release by 2.027, 1.243, and 1.463 kJ·g⁻¹, respectively. Compared with Fe₃O₄, Co₃O₄ microspheres, V₆O₁₃ nanobelts, and α-Fe₂O₃/C, the M₂O₃/CNTs showed better catalytic activity in the thermal decomposition of AP.

3.2.2. Catalytic Mechanism of Nanocomposites

Moreover, compared with Sm₂O₃/CNTs and Nd₂O₃/CNTs, Y₂O₃/CNTs showed superior catalytic effect in the thermal decomposition of AP. Thermal decomposition peak temperature and the heat release of pure AP and samples are listed in Table 2. From DTA data, the following trend of the total DTA heat release was noticed: pure AP (0.281 kJ·g⁻¹) < f-CNTs + AP (0.627 kJ·g⁻¹) < 2 wt.% Sm₂O₃/CNTs + AP (1.524 kJ·g⁻¹) < 2 wt.% Nd₂O₃/CNTs + AP (1.744 kJ·g⁻¹) < 2 wt.% Y₂O₃/CNTs + AP (2.308 kJ·g⁻¹). This result was consistent with the peak area of these samples.

With the same addition, the obtained Nd₂O₃/CNTs decreased the high decomposition temperature by 123.8°C, which was markedly larger than the decrement with Nd₂O₃/CNTs produced by chemical deposition (93.9°C) [19]. It can be concluded that M₂O₃/CNTs nanocomposites by in situ solvothermal method possessed smaller particle size and higher specific area, which can more effectively catalyze the thermal of decomposition of AP than M₂O₃/CNTs synthesized by chemical deposition.

On the basis of electron transfer theory [28], the presence of partially filled 4d orbital in M³⁺ (M = Y³⁺, Nd³⁺, Sm³⁺) is advantageous for electron transfer [29]. The thermal decomposition of AP was enhanced because the positive hole in M³⁺ can accept electrons from the AP ion and its intermediate products. Moreover, the open pore structure of f-CNTs facilitates electron transfer and heat conduction [30] and can promote the thermal decomposition of AP. By contrast, M₂O₃ nanoparticles with relatively small size and good dispersibility, which enhance catalytic effect, are synthesized on f-CNTs by in situ solvothermal method.

4. Conclusions

M₂O₃/CNT (M = Y, Nd, Sm) nanocomposites were prepared through in situ solvothermal method, and M₂O₃ nanoparticles were successfully attached to f-CNTs. This method can be applied in the preparation of other metal oxide/CNTs nanocomposites. The M₂O₃/CNTs nanocomposites by in situ solvothermal method possessed smaller particle size and higher specific area and decreased the aggregation of M₂O₃ nanoparticles, which can more effectively catalyze the thermal decomposition of AP than M₂O₃/CNTs synthesized by chemical deposition. In addition, compared with Nd₂O₃/CNTs and Sm₂O₃/CNTs, Y₂O₃/CNT composites decreased the high thermal decomposition temperature of AP by 125.5°C, which exhibited the best catalytic performance.

Data Availability

The data used to support the findings of this study are available from the corresponding author upon request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

This work was supported by the sponsorship of Nanjing Key Laboratory of Optometric Materials and Technology, Jiangsu Overseas Research & Training Program for University Prominent Young & Middle-Aged Teachers and Presidents, the research grants from the Natural Science Fund of Jiangsu Province (no. BK20130094), and the Enterprise-Universities Cooperative Innovation Fund of Jiangsu Province (no. BY2014016).

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Copyright © 2018 Xiaojuan Zhang and Lingyun Hao. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Journal of Nanomaterials

Preparation and Catalytic Activity of M2O3/CNTs (M = Y, Nd, Sm) Nanocomposites by Solvothermal Process

Abstract

1. Introduction

2. Experimental

2.1. Materials

2.2. Synthesis of M2O3/CNTs Nanocomposites (M = Y, Nd, Sm)

2.3. Catalytic Activity Measurement

2.4. Characterization

3. Results and Discussion

3.1. Materials Characterization

3.1.1. IR Analysis

3.1.2. XRD Analysis

3.1.3. SEM Analysis

3.1.4. EDS Analysis

3.1.5. TEM Analysis

3.1.6. BET Analysis

3.2. Catalytic Properties

3.2.1. DTA Analysis

3.2.2. Catalytic Mechanism of Nanocomposites

4. Conclusions

Data Availability

Conflicts of Interest

Acknowledgments

References

Copyright

Preparation and Catalytic Activity of M₂O₃/CNTs (M = Y, Nd, Sm) Nanocomposites by Solvothermal Process

2.2. Synthesis of M₂O₃/CNTs Nanocomposites (M = Y, Nd, Sm)