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Communication

Enhanced Catalytic Effect of Ti2CTx-MXene on Thermal Decomposition Behavior of Ammonium Perchlorate

by
Jingxiao Li
1,*,
Yulei Du
2,*,
Xiaoyong Wang
1 and
Xuge Zhi
1
1
School of Mechanical Engineering, Nanjing Vocational University of Industry of Technology, Nanjing 210023, China
2
School of Mechanical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China
*
Authors to whom correspondence should be addressed.
Materials 2023, 16(1), 344; https://doi.org/10.3390/ma16010344
Submission received: 9 December 2022 / Revised: 26 December 2022 / Accepted: 27 December 2022 / Published: 30 December 2022
(This article belongs to the Special Issue Ceramic Materials: Processing, Properties and Applications)
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Abstract

:
Transition metal carbonitrides (MXenes) are promising catalysts due to their special structures. Recently, many studies have shown that MXenes have a catalytic effect on the thermal decomposition of ammonium perchlorate (AP). However, the catalytic effects have not been extensively investigated. Therefore, it is important to illustrate the catalytic mechanisms of pure MXene in AP thermal decomposition. Herein, the catalytic properties of Ti2CTx for ammonium perchlorate (AP) thermal decomposition were investigated by numerous catalytic experiments. The results showed that the high-temperature decomposition (HTD) decreased by 83 °C, and the decomposition heat of AP mixed with Ti2CTx increased by 1897.3 J/g. Moreover, the mass spectrum (MS) data showed that the NH3, H2O, O2, N2O, NO, HCl, and NO2 were formed. In addition, according to the X-ray diffraction (XRD), Raman spectrum, high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and X-ray photoelectron spectra (XPS) results, the Ti2CTx nanosheets can adsorb the gaseous products and react with them in-situ, generating anatase-TiO2 and carbon layers. The Ti2CTx, as-resulted anatase-TiO2, and carbon can synergize and further catalyze the thermal decomposition of AP when both electron and proton transfers are accelerated during AP decomposition.

1. Introduction

MXenes, a new group of two-dimensional (2D) early transition metal carbonitrides, are synthesized from the etching of the A layers from Mn+1AXn phases. In this formula, M stands for an early transition metal; A stands for A-group elements; X stands for carbonitrides; and n is 1, 2, or 3 [1,2]. Notably, with the termination of O, OH, and/or F groups on the surface of MXene, Mn+1XnTx becomes more accurate to describe the MXene, where Tx stands for the surface terminations [2]. Due to its good electrical conductivity, large inner surface area, abundant surface terminations, and graphene-like morphology, MXene has been increasingly investigated as a potential material for sensors [3], lithium-ion batteries [4,5], supercapacitors [6,7], metal adsorption materials [8], catalysts [9,10], etc.
Ammonium perchlorate (NH4ClO4, AP) is one of the important oxidative and energetic materials in solid rocket propellants, which provides a powerful thrust to rockets by releasing a large amount of heat and gases [11]. Therefore, to improve the performance of AP thermal decomposition, various catalysts including metals [12], metal oxides [13,14], carbon or carbon-based materials [15,16], and so on, have been exploited for many decades. Recently, due to their large surface area, special 2D layered structure, and excellent electrical conductivity, MXenes also have been used directly as catalysts or ideal substrates to support nanoparticles in boosting the thermal decomposition or burning of AP [17,18,19,20,21]. For instance, by high-temperature heating, Gao and his co-workers prepared MXene-Cu2O composites [18]. Afterward, the as-resulted hybrids were found to greatly influence the thermal decomposition of AP, decreasing its HTD temperature to 121.4 °C. Similarly, Li et al. [19] have reported MXene as a matrix for constructing MXene/MnCo2O4.5 composites with 3D flower-like structures by a hydrothermal process. Simultaneously, MXene/MnCo2O4.5 composites also showed high catalytic activity for AP decomposition. Alternatively, the surface of MXene nanosheets mentioned later could be oxidized during the high-temperature preparation process. Therefore, to prevent MXene from being oxidized, Tan and co-workers [20] fabricated MXene/NiO composites through in-situ precipitation at room temperature and calcination in N2. The compound was highly active in the thermal decomposition of AP, giving an HTD temperature reduction value of 50.6 °C, which was higher than that of NiO alone. Likewise, to protect the surface metal atoms of MXene from oxidation, Zhu and co-workers coated carbonaceous materials on the surface of MXene to construct MXene@C first before the preparation of MnO2/MXene [21]. These MnO2/MXene@C hybrids have greatly accelerated the thermal decomposition of AP, reducing the high-temperature decomposition by 128.8 °C. These studies have shown that adding MXene and MXene-based materials can facilitate the thermal decomposition of AP. However, the effects of MXene on the catalyzation of AP decomposition have not been extensively investigated.
MXenes are sensitive to gases owing to their 2D special structures, numerous highly active functional sites, hydrophilic nature, and high surface area. For example, based on first-principle calculations, Ti2CTx was used to test the adsorption behaviors of gases, such as NH3, H2, CH4, CO, CO2, N2, NO2, and O2 [22]. The result revealed that NH3 can be chemisorbed, and the others are physisorbed on the Ti2CTx sheet because of a different adsorption energy. Similarly, other MXenes, such as Ti3C2, Sc2CO2, and Ti2NS2, also can be confirmed to have great potential applications in gas storage by calculating the adsorption energies of gases on them [23,24,25,26]. These adsorption behaviors can affect the progress of MXenes’ catalytic reaction on AP, because gaseous products, such as NH3, N2, NO, NO2, O2, N2O, H2O, Cl2, HClO4, etc., would be generated during AP degradation [27,28,29]. In addition, owing to numerous exposed metal atoms on the surface, MXenes lack resistance to the oxidizing gases above, resulting in an oxidation reaction and generation of transition metal oxides (TMOs)/MXene composites and carbon. Therefore, MXenes involve a series of complex catalytic reaction processes. Based on this, it is imperative to investigate the catalytic mechanisms of pure MXene in AP thermal decomposition.
Compared to multilayered MXenes, their delaminated ones often exhibit better properties [30,31]. However, the delamination of multilayered MXenes into separated flakes requires intercalation steps after the A layers’ etching process. Furthermore, the intercalated species can have a permanent influence on the MXenes, which could introduce additional factors for investigation on the catalytic mechanism. In this work, in order to avoid the introduced factors, a multilayered Ti2CTx MXene was selected to catalyze AP thermal decomposition. Then, the catalytic mechanism of Ti2CTx on the degradation of AP was studied.

2. Materials and Methods

The preparation of Ti2CTx powders has been reported in detail in our previous work [32]. Briefly, the precursor phase Ti2AlC was exposed to aqueous HF (40 wt.%) for 2.5 h at room temperature; then, the as-prepared suspension was cleaned by DI water several times; at last, purified samples were freeze-dried to obtain Ti2CTx flakes. The AP particles were brought from Guoyao and preheated to 60 °C for 24 h in a vacuum oven to remove moisture. Then, a series of weight ratios of Ti2CTx (0, 5 wt.%, 10 wt.%, 20 wt.%, 30 wt.%) were added into AP, accordingly, and ground in an agate mortar for 15 min.
The surface structure, composition, and morphology of samples were analyzed by scanning electron microscope (SEM, Quant 250F, FEI, Hillsboro, OR, USA), X-ray diffraction (XRD, Bruker-AXS D8 Advance, Bruker, Leipzig, Germany) with Cu-Kα radiation ( λ = 1.54178 Å) operated at 40 mA and 40 kV), transmission electron microscope (TEM, JEM-200CX, JEOL, Tokyo, Japan) operated at 200 kV, X-ray photoelectron spectroscopy (XPS, PHI 5000 VersaProbe, Ulvac Phi, Chigasaki, Japan, Al-Kα radiation), and Raman spectroscopy (JY HR800, JY, France, λ = 514 nm).
The catalytic effect of the prepared samples on the thermal decomposition of AP was studied by using an STA449F TG-DSC at heating rates of 5, 10, 20 °C/min, and between 40 and 500 °C. The purge gas used was 99.995% pure Argon. The overall purge flow rate was maintained at 20 mL/min. Simultaneously, a Netzsch (Aeolos QMS403, Selb, Germany) mass spectrometer was used to study the decomposition products.

3. Results and Discussion

3.1. Thermal Decomposition of Pure AP

The morphologies and structures of AP and Ti2CTx were characterized by SEM and XRD, as shown in Figure 1. Figure 1a shows that the AP particles were relatively coarse with various sizes, and in Figure 1b, all diffraction peaks were ascribed to AP, confirming its purity. Figure 1c shows the typical 2D stacked multilayered structure of Ti2CTx. Moreover, the XRD pattern in Figure 1d shows that the diffraction peaks were located at around 9°, which also confirmed the formation of Ti2CTx [33].
Figure 1e shows the TG and DSC curves of pure AP, which reveal that the thermal decomposition of pure AP occurred in three stages. In the first stage, the endothermic peak appeared at 242 °C without weight loss, which is due to the transition from orthorhombic to cubic form [34]. In the second stage (named low-temperature decomposition, LTD), the exothermic peak at 311 °C was assigned to the partial decomposition of AP with 17.5 wt.% weight loss, and some intermediates were formed by dissociation and sublimation. The third peak (high-temperature decomposition, HTD) appeared at a relatively higher temperature of 447 °C, indicating the complete decomposition of the intermediate to volatile products.
For describing the release of volatiles, MS was used to follow the representative mass fragments of the substances produced by AP. As shown in Figure 1f, the evolution profiles of NH2+ (m/z = 16), O+ (m/z = 16), NH3+ (m/z = 17), H2O (m/z = 18), NO (m/z = 30), O2 (m/z = 32), HCl (m/z = 36), N2O (m/z = 44), and NO2+(m/z = 46) along with temperatures were presented with 10 °C min−1 by MS. The curves above show that the main decomposition products in LTD were NH3, H2O, O2, and N2O, indicating that AP was first decomposed into NH3 and HClO4, and HClO4 was further decomposed into oxidizing substances, and then these oxidizing substances reacted with NH3, forming H2O, O2, and N2O. Compared with the LTD stage, the ion current intensity in the HTD stage was higher, suggesting that the decomposition of AP was mainly concentrated in this stage. The broad peak type of each ion flow indicates that the decomposition reaction of pure AP proceeded slowly, in which the NH3, H2O, O2, N2O, NO, HCl, and NO2 were mainly examined. In addition, the formation temperature of HCl complied with that of H2O, but later than other products, which illustrates that HCl is a secondary product.

3.2. The Catalytic Activity of Ti2CTx

Figure 2 shows that the catalytic performance of various ratios’ addition of Ti2CTx on thermal decomposition of AP was tested by DSC and TG. Figure 2a shows the DSC curves of AP in the presence of 0, 5 wt.%, 10 wt.%, 20 wt.%, and 30 wt.% Ti2CTx. As shown, the results indicated that Ti2CTx did not affect the crystal transformation. The changes in peak decomposition temperature on DSC curves and initial decomposition temperature on TG curves (in Figure 2b) show the positively catalytic role of Ti2CTx in the thermal decomposition of AP. With increasing Ti2CTx content, the LTD peak rarely changed, but two exothermic peaks appeared in the HTD stage, and both exothermic peaks moved towards the temperature reduction direction, and finally became a sharp exothermic peak when the additional amount of Ti2CTx was up to 30 wt.%. The HTD temperatures of AP-x wt.% Ti2CTx (x = 5, 10, 20, and 30) mixtures were 435, 415, 385, and 359 °C, respectively, and decreased by 12, 32, 63, and 88 °C compared with pure AP (447 °C), respectively. In addition, the TG curves show that the addition of Ti2CTx affected the initial decomposition temperature of AP, decreasing it by 15 °C when adding 5~20 wt.% Ti2CTx and 35 °C when adding 30 wt.% Ti2CTx, respectively. These results suggest that Ti2CTx has a catalytic effect on the decomposition of both LTD and HTD.
In Figure 2c, the released energies of the mixtures were 1103, 1332, 2087, and 2527 J/g corresponding to AP-x wt.% Ti2CTx (x = 5, 10, 20, 30) mixtures, enhanced by 473.3, 702.3, 1457.3, and 1897.3 J/g compared to 629.7 J/g of pure AP. However, it is obvious that the growth rates of released energies were not always positive, which is probably due to the excessive addition of Ti2CTx-MXene. In addition, as shown in Table 1, MXene-based composites exhibited better catalytic activity when the mixture ratio of the catalyst was low.
Figure 3 demonstrates the MS results of AP in the presence of Ti2CTx (0, 10, and 30 wt.%). AP was completely decomposed at lower temperatures and shorter times. In addition, the results show that the intensity of the ion currents of NO, NO2, H2O, and HCl of AP mixed with Ti2CTx was lower than that of pure AP, suggesting that the layered Ti2CTx easily absorbed the gaseous products. Notably, the intensity of the ion currents of O2 and N2O of Ap-10 wt.% Ti2CTx was higher than that of pure AP, which indicates that the addition of Ti2CTx promoted the formation of the two gases. However, when 30 wt.% Ti2CTx was added, the change trend of the MS results of O2 and N2O complied with that of other ions. This also complies with the previous report [22,24] that Ti2CTx with special structures can adsorb gases and be easily oxidized by oxidizing gases. Therefore, it can be inferred that Ti2CTx could absorb O2 and N2O and react with the two gases. Usually, this phenomenon occurs in the thermal decomposition process of AP catalyzed by transition metals, and the generated transition metal oxides will synergistically catalyze the thermal decomposition of AP [37].

3.3. Catalytic Mechanism of Ti2CTx

To reveal the thermal decomposition mechanism of AP catalyzed by MXene, the Ti2CTx after catalysis was characterized by the SEM, XRD, Raman Spectroscope, XPS, TEM, and HRTEM.
Figure 4a shows the XRD results of the Ti2CTx after the catalytic thermal decomposition of AP. After catalyzing the thermal decomposition of AP from room temperature to 500 °C, peak centers at 25.3°, 36.9°, 37.8°, 48°, 53.9°, 55°, 62.7°, 68.8°, 70°, 75°, and 76° appeared in all the samples, which can respectively be attributed to (101), (103), (004), (200), (105), (211), (204), (116), (220), (215), and (301) planes of anatase-TiO2 (A-TiO2) according to JCPDS 21-1272. The very weak peak at 27.48° belonged to rutile-TiO2 (JCPDS 21-1276), which demonstrates that a little amount of rutile-TiO2 was formed. Three extra peaks located at 35.9°, 42.7°, and 60.5° can be indexed to TiC (JCPDS 65-0242), which were the inevitable intermediate products during Ti2AlC preparation, and it was hard to remove. Notably, the typical peak of Ti2CTx shifted to a lower angle. Based on these results, A-TiO2 particles were formed during the catalytic process, which paralleled heating MXenes in the air or other atmospheres [38,39]. The formation of A-TiO2 was further explained by the Raman results (shown in Figure 4b). After the thermal decomposition catalyzed by AP, four peaks centered at 144, 399, 519, and 639 cm−1 appeared, which responded well to the vibrational modes Eg(1), B1g(1), A1g, and Eg(3) of anatase (A-TiO2), respectively [40]. Meanwhile, relatively weak D- and G-bands were observed (shown in the inset of Figure 4b), indicating that only a small amount of carbon was formed on the surface of Ti2CTx nanosheets with the formation of A-TiO2.
Figure 5 shows XPS patterns of the surface and inner (after 10 s Ar sputtering) of samples after the catalytic thermal decomposition of AP. The fitting components are listed in Table 2. On the sample surfaces, almost 79% of the Ti 2p region belonged to TiO2, and 38% of the O 1s region belonged to TiO2. However, after 10 s Ar sputtering, the percentage of the Ti 2p region and O 1s region decreased to 3% and 7%, respectively. This suggested that the Ti atoms on the surface of the Ti2CTx nanosheets were oxidized to TiO2 during the process of accelerating the exothermic decomposition of AP. The interior structures of the Ti2CTx were still maintained. These results demonstrated that the C-Ti bonds were broken, forming TiO2 particles and carbon layers. Additionally, there were still numerous C-Ti-Tx bonds [41], and the carbon layers stuck the TiO2 particles on the surface of Ti2CTx like “glue”, which was helpful to maintain the stability of Ti2CTx.
The SEM image (Figure 6a,b) shows that the interlamellar spacing of Ti2CTx became larger after the catalytic thermal decomposition of AP. This amplification was partially due to A-TiO2 formation on the external surface, and presumably also between the layers. However, no typical A-TiO2 particles were observed from the SEM image. Therefore, further confirmation was conducted by the TEM analysis. The TEM image (Figure 6c) and HRTEM image (Figure 6d) demonstrated that some Ti2CTx nanosheets still retained their planar structure, while others transformed into small crystalline particles. The calculated d-spacing values of the latter phase agreed with values for anatase in the JCPDS card (21-1272). The indexed SAED pattern (shown in Figure 6e), taken from the square region, combined two phases: the original Ti2CTx and anatase-TiO2. Herein, it is also clear that Ti2CTx underwent surface oxidation when the catalytic exothermic decomposition of AP happened.
Generally, there are two main viewpoints on the mechanism of the thermal decomposition of AP (NH4ClO4)–electron transfer and proton transfer–and the process is usually as follows:
(1)
electrons (e−) transfer from ClO4− to NH4+:
ClO4− NH4+ → ClO4 + NH4
(2)
protons (H+) transfer from NH4+ to ClO4−:
ClO4− NH4+ →HClO4 + NH3
In the actual thermal decomposition process of AP, both of these mechanisms may occur, but the occurrence and degree of occurrence will vary under different induced environments. According to the previous results, it can be considered that the mechanism of Ti2CTx catalyzed the thermal decomposition of AP in the following aspects.
First, XPS results show that the Ti element in Ti2CTx presented multiple valence states. In Rudloff’s report [51], the catalytic effect of transition metal oxides on the thermal decomposition of AP may be attributed to their multivalent change, which can result in the acceleration of electrons’ migration from ClO4− to NH4+ during the redox process, thus boosting the entire decomposition reaction. Here, Ti atoms on the surface of Ti2CTx are transition metals, and their 3d orbits are electron-unsaturated, where the empty obits could provide convenient bridges for electron transfer. In addition, Ti3+ ions possess separate d electrons in the valence band, which could provide more convenient tunnels for electron movement. Herein, the interaction between Ti2CTx and AP could contribute to thermal decomposition, forming NH3 and HClO4.
NH4+ ClO4− → NH3(a) + HClO4(a) → NH3(g) + HClO4(g)
Second, the special layered structure endows Ti2CTx with good gas adsorption performance. Based on the first-principle calculation, Yu and co-workers [22] found that the Ti2CO2 (Tx = O2) can selectively adsorb NH3(g), and the process is reversible, wherein the NH3(g) could be desorbed after the strain of Ti2CO2 releasing. Accordingly, when the NH3(g) is formed during the decomposition of AP, it can easily be adsorbed by Ti2CTx nanosheets. Thus, the MS results confirmed that no NH3(g) signal was detected when Ti2CTx nanosheets were added. Accordingly, the adsorption behavior of Ti2CTx nanosheets can reduce the concentration of decomposition products, promote thermal decomposition, and provide a place for the oxidation of NH3. Moreover, the MS result further confirmed the adsorption ability of Ti2CTx, showing that the concentration of the resulting H2O, O2, and N2O gases with Ti2CTx addition was lower than that of pure AP, which is important to catalyze thermal decomposition.
Third, as can be seen from the XRD and TEM results above, TiO2 was formed when oxidizing gases were emitted by AP decomposition, as follows:
Ti2CTx + O2 → TiO2+ Carbon + other products
Ti2CTx + N2O → TiO2 + Carbon + other products
Ti2CTx + H2O → TiO2 + Carbon + other products
In addition, the formation of TiO2 could reduce the concentration of gaseous products. Generally, carbon layers and Ti3+ ions are formed with the formation of anatase-TiO2 particles. Meanwhile, these TiO2 particles can prevent Ti2CTx from further oxidation and participate in the catalytic reaction as transition metal oxides [52].
Fourth, some electrons would be generated from the semiconductor Ti2CTx (Tx = OH and O) and the resulting anatase-TiO2 when they are excited by thermal energy. These excited electrons alongside electrons transferring from NH4+ to ClO4− would interact with HClO4 adsorbed on the surface of Ti2CTx layers to form superoxide ion O2− [53], then oxidize NH3 into H2O, NO, NO2, N2O, and so on [54,55]. Importantly, NH3 oxidation is a strongly exothermic reaction, thus increasing the exothermic heat of the reaction.
4 NH3 + 5 O2 = 4 NO + 6 H2O ΔH = 905.9 kJ/mol
4 NH3 + 7 O2 = 4 NO2 + 6 H2O ΔH = 282.8 kJ/mol
4 NH3 + 4 O2 = 2 N2O + 6 H2O ΔH = 1104.9 kJ/mol
Furthermore, MXenes have excellent thermal conductivity [56]; therefore, the heat conduction rate of the whole reaction system would be significantly improved by the Ti2CTx addition.
Based on the abovementioned results and analysis, as Figure 7 shows, the thermal decomposition mechanism of AP catalyzed by Ti2CTx is described as follows: above all, Ti2CTx, TiO2, and carbon layers with excellent electron conductivity could boost the transfer of electrons (e−) from ClO4− to NH4+, promoting decomposition of NH4ClO4 and the formation of HClO4 and NH3; meanwhile, the Ti2CTx nanosheets can adsorb gaseous products, reduce the concentration of products, and increase the contact chance of HClO4 and NH3, and shorten the reaction path as well; the formation of TiO2 could also reduce the concentration of gaseous products, accelerating the decomposition; then, excited electrons (e−) generated from the semiconductor Ti2CTx (x = -OH and = O) and resulting TiO2 when they are heated, would be transmitted to HClO4, the formation of superoxide O2−, which could oxidize the NH3 to produce the final products and release significant amounts of heat; finally, MXene has good thermal conductivity, which can conduct heat quickly and promote a reaction.

4. Conclusions

In conclusion, the Ti2CTx showed an enhanced catalytic effect on AP thermal decomposition. The thermal decomposition temperature of the composite decreased by 15, 28, 65, and 83 °C corresponding to 5, 10, 20, and 30 wt.% additives, respectively. X-ray diffraction (XRD) and Raman spectroscopy results showed anatase-TiO2 formation during the exothermic decomposition process. The high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and XPS results demonstrated that anatase-TiO2 were uniformly distributed on the surface of Ti2CTx. Based on these results, a possible catalytic mechanism for the thermal decomposition of AP catalyzed by Ti2CTx was proposed, which would be beneficial for understanding the catalytic mechanism of MXenes and developing efficient catalysts.

Author Contributions

Conceptualization, J.L.; methodology, J.L. and Y.D.; validation, Y.D., X.W. and X.Z.; investigation, J.L.; writing—original draft preparation, J.L. and Y.D.; writing—review and editing, Y.D. and J.L.; supervision, Y.D.; project administration, Y.D. All authors have read and agreed to the published version of the manuscript.

Funding

The Natural Science Foundation of the Jiangsu Higher Education Institutions of China (grant number 21KJB430040), Start-up Fund for New Talented Researchers of Nanjing Vocational University of Industry Technology (grant numbers YK19-01-07, YK19-01-08).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Materials 16 00344 g001 550
Figure 1. (a) SEM image and (b) XRD of AP; (c) SEM image and (d) XRD of Ti2CTx; (e) DSC and TG curves for the thermal decomposition of AP; (f) ion intensity curves of pure AP during the thermal decomposition.
Figure 1. (a) SEM image and (b) XRD of AP; (c) SEM image and (d) XRD of Ti2CTx; (e) DSC and TG curves for the thermal decomposition of AP; (f) ion intensity curves of pure AP during the thermal decomposition.
Materials 16 00344 g001
Materials 16 00344 g002 550
Figure 2. (a) DSC, (b) TG curves, and (c) heat release of pure AP and AP-x wt.%Ti2CT (x = 5, 10, 20, 30 wt.%).
Figure 2. (a) DSC, (b) TG curves, and (c) heat release of pure AP and AP-x wt.%Ti2CT (x = 5, 10, 20, 30 wt.%).
Materials 16 00344 g002
Materials 16 00344 g003 550
Figure 3. Ion intensity curves of (a) H2O+, (b) NO+, (c) O2+, (d) HCl+, (e) N2O+, and (f) NO2+. The black curves, red curves, and blue curves stand for decomposition products of pure AP, AP-10% Ti2CTx, and AP-30% Ti2CTx, respectively.
Figure 3. Ion intensity curves of (a) H2O+, (b) NO+, (c) O2+, (d) HCl+, (e) N2O+, and (f) NO2+. The black curves, red curves, and blue curves stand for decomposition products of pure AP, AP-10% Ti2CTx, and AP-30% Ti2CTx, respectively.
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Materials 16 00344 g004 550
Figure 4. (a) XRD patterns and (b) Raman spectra of Ti2CTx after catalytic thermal decomposition of AP. a, b, c, d stand for Ti2CTx after catalytic thermal decomposition of AP in AP-x wt.%Ti2CTx (x = 5, 10, 20, 30 wt.%) samples, respectively. The signs “*” and “#” stand for anatase and rutile, respectively. D and G stand for D-band and G-band of carbon, respectively.
Figure 4. (a) XRD patterns and (b) Raman spectra of Ti2CTx after catalytic thermal decomposition of AP. a, b, c, d stand for Ti2CTx after catalytic thermal decomposition of AP in AP-x wt.%Ti2CTx (x = 5, 10, 20, 30 wt.%) samples, respectively. The signs “*” and “#” stand for anatase and rutile, respectively. D and G stand for D-band and G-band of carbon, respectively.
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Materials 16 00344 g005 550
Figure 5. Component peak fitting of XPS spectra for Ti2CTx after catalytic thermal decomposition of AP, (a) Ti 2p, (b) C 1s, and (c) O 1s on the surface, and (d) Ti 2p, (e) C 1s, and (f) O 1s in the inner (after 10 s Ar sputtering).
Figure 5. Component peak fitting of XPS spectra for Ti2CTx after catalytic thermal decomposition of AP, (a) Ti 2p, (b) C 1s, and (c) O 1s on the surface, and (d) Ti 2p, (e) C 1s, and (f) O 1s in the inner (after 10 s Ar sputtering).
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Materials 16 00344 g006 550
Figure 6. FESEM image of Ti2CTx after decomposition of AP (a) AP-5 wt.%Ti2CTx, (b) AP-10 wt.%Ti2CTx, (c) AP-20 wt.%Ti2CTx, and (d) AP-30 wt.%Ti2CTx. (e) TEM image of Ti2CTx after decomposition of AP and its (f) high-resolution TEM image, as well as (g) SEAD patterns. “A” stands for anatase-TiO2.
Figure 6. FESEM image of Ti2CTx after decomposition of AP (a) AP-5 wt.%Ti2CTx, (b) AP-10 wt.%Ti2CTx, (c) AP-20 wt.%Ti2CTx, and (d) AP-30 wt.%Ti2CTx. (e) TEM image of Ti2CTx after decomposition of AP and its (f) high-resolution TEM image, as well as (g) SEAD patterns. “A” stands for anatase-TiO2.
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Materials 16 00344 g007 550
Figure 7. Schematic shows the catalytic mechanism of thermal decomposition of AP by Ti2CTx.
Figure 7. Schematic shows the catalytic mechanism of thermal decomposition of AP by Ti2CTx.
Materials 16 00344 g007
Table
Table 1. Comparison of catalytic activity for AP by MXenes and their composites.
Table 1. Comparison of catalytic activity for AP by MXenes and their composites.
Materials Content (wt.%) Reduction in HTD Temperature ( °C ) Increase in Decomposition Heat (J/g) Reference
Ti2CTx 30 83 1897.3 This work
MXene(Ti3C2Tx) 2 12.4 - [18]
MXene/Cu2O 121.4
MXene/MnCo2O4.5 4 131.7 1132.4 [19]
MXene(Ti3C2Tx) 2 10.2 - [20]
MXene/NiO 50.6
MnO2/MXene(Ti3C2Tx) 2 128.8 - [21]
MXene (Ti3C2Tx) 2 28.1 49.5 [35]
Co3O4@MXene 108.9 1162.7
MXene (Ti3C2Tx) 2 38.8 73.6 [36]
MXene/ZnCo2O4 138.3 1079.2
Note: In this table, HTD represents the high-temperature decomposition.
Table
Table 2. XPS peak fitting results for Ti2CTx after catalyzing AP on the surface and inner locations (after 10 s Ar+ sputtering). Numbers in brackets in column 3 are peak locations, and their full widths at half maximum, FWHM, are listed in column 4 in brackets.
Table 2. XPS peak fitting results for Ti2CTx after catalyzing AP on the surface and inner locations (after 10 s Ar+ sputtering). Numbers in brackets in column 3 are peak locations, and their full widths at half maximum, FWHM, are listed in column 4 in brackets.
LocationRegionBE [eV]FWHM [eV]FractionAssigned to Reference
SurfaceTi 2p3/2
(2p1/2)		457.2 (462.9)2.1 (2.1)0.21Ti3+[42]
458.6 (464.2)0.9 (1.0)0.79TiO2[43,44]
O 1s529.91.00.38TiO2[41,44]
531.21.40.18C-Ti-Ox[41,45]
532.01.10.40C-Ti-(OH)x[41,45]
532.81.20.01Al2O3[45,46,47]
533.82.00.03H2Oads[41,45]
C 1s2821.00.38C-Ti-Tx[42,48]
284.71.60.52C-C[49]
286.31.40.10CHx/C-O[49]
Inner (after 10 s sputtering)Ti 2p3/2
(2p1/2)		454.8 (461.0)1.0 (1.9)0.32Ti[42,48]
455.9 (461.5)2.2 (2.4)0.20Ti2+[42]
457.5 (463.2)2.3 (2.0)0.41Ti3+[42]
459.0 (464.7)1.0 (1.1)0.03TiO2[43,44]
460.4 (466.1)2.1 (2.9)0.04C-Ti-Fx[50]
O 1s530.31.10.07TiO2[41,44]
531.21.20.38C-Ti-Ox[41,45]
531.91.10.51C-Ti-(OH)[41,45]
533.71.70.04H2Oads[41,45]
C 1s282.00.60.69C-Ti-Tx[42,48]
284.61.80.30C-C[49]
286.51.40.01CHx/C-O[49]
F 1s685.21.80.41C-Ti-Fx[50]
686.21.60.31AlFx[46]
687.32.50.28Al(OF)x[46]
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Li, J.; Du, Y.; Wang, X.; Zhi, X. Enhanced Catalytic Effect of Ti2CTx-MXene on Thermal Decomposition Behavior of Ammonium Perchlorate. Materials 2023, 16, 344. https://doi.org/10.3390/ma16010344

AMA Style

Li J, Du Y, Wang X, Zhi X. Enhanced Catalytic Effect of Ti2CTx-MXene on Thermal Decomposition Behavior of Ammonium Perchlorate. Materials. 2023; 16(1):344. https://doi.org/10.3390/ma16010344

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Li, Jingxiao, Yulei Du, Xiaoyong Wang, and Xuge Zhi. 2023. "Enhanced Catalytic Effect of Ti2CTx-MXene on Thermal Decomposition Behavior of Ammonium Perchlorate" Materials 16, no. 1: 344. https://doi.org/10.3390/ma16010344

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