Research on regulating thermal decomposition of ammonium perchlorate by Fe-based functional coordination polymers

Research on regulating thermal decomposition of ammonium perchlorate by Fe-based functional coordination polymers | Authorea try { document.documentElement.classList.add('js'); } catch (e) { } var _gaq = _gaq || []; _gaq.push(['_setAccount', 'G-8VDV14Y67G']); _gaq.push(['_trackPageview']); (function() { var ga = document.createElement('script'); ga.type = 'text/javascript'; ga.async = true; ga.src = ('https:' == document.location.protocol ? 'https://ssl' : 'http://www') + '.google-analytics.com/ga.js'; var s = document.getElementsByTagName('script')[0]; s.parentNode.insertBefore(ga, s); })(); Skip to main content Preprints Collections Wiley Open Research IET Open Research Ecological Society of Japan All Collections About About Authorea FAQs Contact Us Quick Search anywhere Search for preprint articles, keywords, etc. Search Search ADVANCED SEARCH SCROLL This is a preprint and has not been peer reviewed. Data may be preliminary. 23 December 2025 V1 Latest version Share on Research on regulating thermal decomposition of ammonium perchlorate by Fe-based functional coordination polymers Authors : Yan Zhao , Bian Li , Guixi Liu , Tao Zhang , Xiaoyu Lv , Chaohui Guo , Jiexin Weng , Zhou Xing 0000-0002-9980-1937 [email protected] , Shuo Liu , and Zhongyun Ma Authors Info & Affiliations https://doi.org/10.22541/au.176647887.75816487/v1 212 views 49 downloads Contents Abstract Supplementary Material Information & Authors Metrics & Citations View Options References Figures Tables Media Share Abstract The present research investigates the regulation of ammonium perchlorate’s (AP) thermal decomposition through Fe-CPs@AP energetic composites. The propellant formulations incorporating 4wt% Fe-CPs@AP catalyst display superior combustion characteristics, achieving 36-43% enhancement in burning rates compared to control samples while maintaining a remarkably low pressure exponent of 0.571. The enhanced performance originates from the optimized interfacial interaction between Fe-CPs@AP and propellant matrices, facilitating the formation of in-situ generated uniformly dispersed metal oxide nanoparticles that maximize catalytic efficiency during AP decomposition. The mechanistic study and DFT calculation show that Fe-containing components and catalytic centers act as mediators. They facilitate electron transport during the LTD phase, optimize electron transfer between ClO 4 - and NH 4 + , help adsorb oxygen species, boost thermal energy release in the high-temperature stage, and improve AP breakdown efficiency. The energetic material simultaneously addresses multiple challenges including AP’s hygroscopic tendencies, particle aggregation phenomena, and sensitivity to pressure variations. This study provides theoretical insights and practical applications for developing high-efficiency combustion propellant systems. Research on regulating thermal decomposition of ammonium perchlorate by Fe-based functional coordination polymers Yan Zhao, +[ a,b ] , Bian Li, +[ a ] Guixi Liu, [ b ] * Tao Zhang [ b ] , Xiaoyu Lv [ b ] , Chaohui Guo [ b ] , Jiexin Weng, [ b ] * Xing Zhou , [ a ] * , Shuo Liu [c] , Zhongyun Ma [d] To Chin. J. Chem. (Article) * Corresponding author. College of Aerospace Science and Technology, National University of Defense Technology, Changsha 410073, P. R. China. E−mail: [email protected] + These authors contributed to the work equally and should be regarded as co-first authors. a College of Aerospace Science and Technology, National University of Defense Technology, Changsha 410073, P. R. China. b Power Machinery Institute of Inner Mongolia, Hohhot 010010, P. R. China. c College of Computer Science and Technology, Huaqiao University, Xiamen 361021, P. R. China. d College of Chemistry of Xiangtan University, Xiangtan, 411105, P. R. China. Supporting information for this article is available on the WWW under http://doi.org/10.1002/cjoc. or from the author. Keywords Fe-based functional coordination polymers; AP-HTPB propellant; Burning catalyst; Adjustable decomposition of AP. Comprehensive Summary The present research investigates the regulation of ammonium perchlorate’s (AP) thermal decomposition through Fe-CPs@AP energetic composites. The propellant formulations incorporating 4wt% Fe-CPs@AP catalyst display superior combustion characteristics, achieving 36-43% enhancement in burning rates compared to control samples while maintaining a remarkably low pressure exponent of 0.571. The enhanced performance originates from the optimized interfacial interaction between Fe-CPs@AP and propellant matrices, facilitating the formation of in-situ generated uniformly dispersed metal oxide nanoparticles that maximize catalytic efficiency during AP decomposition. The mechanistic study and DFT calculation show that Fe-containing components and catalytic centers act as mediators. They facilitate electron transport during the LTD phase, optimize electron transfer between ClO 4 - and NH 4 + , help adsorb oxygen species, boost thermal energy release in the high-temperature stage, and improve AP breakdown efficiency. The energetic material simultaneously addresses multiple challenges including AP’s hygroscopic tendencies, particle aggregation phenomena, and sensitivity to pressure variations. This study provides theoretical insights and practical applications for developing high-efficiency combustion propellant systems. Background and Originality Content Currently, hydroxyl-terminated polybutadiene (HTPB) composite solid propellant, which employs ammonium perchlorate as the oxidizer and aluminum powder (Al) as the metallic fuel, remain the predominant choice in global solid propulsion systems. Within these energetic compositions, oxidizers constitute the principal component mass fraction exceeding 60% [1-3] . AP demonstrates distinct advantages over alternative oxidizers, exhibiting superior oxidative potential, elevated gas production efficiency, economic viability, substantial active oxygen content, and excellent compatibility with binder systems [4] . The combustion characteristics of propellants are fundamentally governed by AP’s thermal decomposition parameters including initiation temperature, reaction kinetics, and enthalpy variations [5] . Catalytic modification of these decomposition properties presents an effective strategy for enhancing propellant combustion efficiency. Numerous studies have confirmed that combustion modifiers significantly influence the regulatory mechanisms governing solid propellant combustion behavior [6,7] . Generally speaking, combustion catalysts that have been intensively investigated encompass metallic substances and their oxides [8,9] , inorganic metallic salts [10] , organometallic compounds [11] , carbon-based nanomaterial combustion accelerators [12] , and various energetic combustion catalysts [13,14] . The addition of conventional combustion velocity catalysts can elevate the oxidizer’s thermal decomposition rate. Classical combustion catalysts are characterized by relatively economical manufacturing expenses and accessible technical requirements. Nevertheless, their efficacy in augmenting the combustion speed is circumscribed. Concurrently, ultrafine processing of ammonium perchlorate frequently plays a pivotal role in boosting propellant combustion efficiency. Nevertheless, nanoscale ammonium perchlorate particles display non-uniform morphological characteristics accompanied by challenges including particle aggregation tendencies and elevated sensitivity levels. These technical limitations substantially impact the manufacturing feasibility, operational safety, and functional performance of propellant systems. Composite nanoenergetic materials functioning as combustion catalysts offer viable solutions to these issues. By implementing strategic nanostructuring of AP with catalytic components, this approach maximizes interfacial contact between oxidizer and catalyst particles, consequently enhancing redox reaction kinetics [15,16] . Such engineered nanomaterials demonstrate capacity for extending the adjustable combustion rate spectrum of solid propellants while improving flame consistency, ultimately enabling tailored regulation of combustion characteristics through optimized energy release mechanisms [17] . Coordination polymers (CPs) represent a type of crystalline materials, which display a wide array of topologies and uniform pores of specific dimensions. They are synthesized through the combination of isolated metal centers or polynuclear clusters with bi/multidentate linkers [18] . Transition metals are commonly chosen as coordination centers to enhance catalytic performance and provide primary reactive centers for chemical transformations. Nitrogen-rich organic ligands with elevated energy potential are typically employed in their construction [19] . The adaptability of metallic nodes and bridging ligands, combined with their diverse coordination geometries, allows precise tuning of energetic CP properties [20,21] . Notably, these materials possess extensive surface areas, ordered nanoporous networks [22] , and atomically dispersed catalytic sites. Such characteristics facilitate the adsorption of perchloric acid and ammonia gases during the thermal decomposition process of AP, positioning CPs as promising candidates for advanced solid propellant formulations. Feng et al. [23] carried out an in-depth investigation of ferrocene-based transition coordination polymers. In this study, 1,1’-ferrocenedicarboxylic acid (FcDA) was employed as a linker. The resulting CPs were designated as M-FcD-MOFs, characterized by expansive surface areas and superior thermal stability. Significantly, they can decrease the high-temperature decomposition peak temperature by 90 °C and reduce the apparent activation energy by 20.4%. Moreover, they can enhance the apparent heat release of AP by 1082 Jg -1 . Comparative studies reveal that metal oxides formed during CPs’ decomposition exhibited superior catalytic efficiency compared to conventional metal oxide catalysts [24,25] , with in-situ generated nanoparticles showing particularly enhanced activity in thermal decomposition processes. Our research group has achieved the successful synthesis of a diverse range of monometallic coordination polymers for use as combustion catalysts, with Fe5B [26] and ZIF-67 being notable examples. The HTD peak temperatures of these nanoparticles were found to decrease to 297.4 °C and 321.9 °C, individually. Building upon these results, we intend to conduct further investigations into the impact of Fe-CPs@AP with varying contents on the burning rate of the propellant. This research strategically selects Fe ions as highly reactive transition metal components alongside 2-methylimidazole, a nitrogen-dense polyazaheterocyclic ligand, for constructing coordination polymer frameworks. Through controlled integration of ammonium perchlorate into the nanoarchitectured Fe-based coordination polymer matrix, novel composite energetic materials with enhanced properties have been successfully developed. Detailed analysis reveals the concentration-dependent impact of Fe-CPs@AP composites on the combustion velocity of the propellant under pressure conditions spanning from 3.0 to 9.0 MPa. This is concurrently accompanied by a comprehensive evaluation of the complete combustion characteristics and an in-depth elucidation of the thermal degradation pathways. The combustion acceleration mechanism and DFT calculation primarily target the precise modulation of AP’s catalytic degradation processes while resolving technical obstacles concerning ultrafine AP’s hygroscopic tendencies and particle coalescence. 2. Experimental Section 2.1 Materials Ultrafine ammonium perchlorate (D50≈1 μm) was acquired from Tianyuan New Material Technology Co., Ltd. Fe(NO 3 ) 3 9H 2 O and 2-Methylimidazole (analytical purity) were supplied by Shanghai Aladdin Biochemical Technology Co., Ltd. Additional reagents including methanol, acetone, and dichloromethane (analytical grade) originated from the Shanghai Institute of Organic Chemistry. The binder system comprised hydroxy-terminated polybutadiene (HTPB), while Toluene diisocyanate (TDI) served as curing agent, Dioctyl sebacate (DOS) as plasticizer, and Methyl apoxide (MAPO) as cross-linking agent, all procured from Sinopharm Group. Unless specifically noted, chemical substances were utilized without further purification. 2.2 Preparation of Fe-CPs powder catalysts The Fe-CPs powder catalysts were synthesized by co-precipitation. A methanolic solution containing Fe(NO 3 ) 3 9H 2 O (4.0 g, 9.9 mmol) in 30 mL solvent was combined with 30.0 mL of methanol containing 2-methylimidazole (5.0 g, 52 mmol). The resultant mixture was completely dissolved and mechanically agitated for 10 minutes at ambient temperature using a 100-mL reaction vessel. During this mixing process, 1.0 mL of 1.0 M sodium hydroxide solution was gradually introduced. The obtained precipitate underwent vacuum filtration followed by triple washing with 10 mL aliquots of methanol, then subjected to natural drying at room temperature for 48 hours. 2.3 Preparation of Fe-CPs@AP Fe-CPs@AP energetic composites were synthesized through a solvent-nonsolvent strategy. This process entailed depositing ultrafine ammonium perchlorate coating onto Fe-based coordination polymers. Acetone served as the solvent medium while dichloromethane acted as the antisolvent component. Initially, 0.1 g of newly synthesized Fe-CPs was uniformly dispersed in 200.0 mL dichloromethane through probe-type ultrasonic homogenization (Ultrasonic horn diameter: ∅10; Output power: 200 W; Operating frequency: 20 kHz) to prepare a solution. Subsequently, 0.3 g of ultrafine AP was completely dissolved in 100.0 mL of acetone to form homogeneous AP-acetone solution. The Fe-CPs suspension was then gradually introduced into the AP-containing solution under ambient conditions. The mixture was vigorously stirred at a rotational speed of 600 r/min for 30 minutes. The resultant Fe-CPs@AP nanocomposites were subsequently vacuum-filtered and air-dried at 25°C. For comparison, a simple physical mixture of 0.10 g of Fe-CPs and 0.30 g of ultrafine AP was designated as Fe-CPs/AP. 2.4 Characterization Crystal structure analysis was acquired via X-ray diffraction (XRD, Bruker D8 Advance, Cu-Kα, 2θ ranging from 5° to 90°). Material morphology was characterized using scanning electron microscopy (SEM, TESCAN MIRA LMS). The elemental compositions of Fe-CPs@AP were determined by Energy Dispersive X-ray Spectrometry (EDAX). Molecular vibration characteristics were examined through Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR, PerkinElmer Spectrum 3, in the range of 4000 cm -1 -500 cm -1 ). The surface chemical components were analyzed by X-ray photoelectron spectroscopy (XPS, Thermo Scientific K-Alpha). Thermal behavior evaluation involved simultaneous TG-DSC measurements (Beijing Henven Scientific Instrument) under nitrogen atmosphere (40 mL/min flow rate), with 3 ± 0.5 mg samples in alumina crucibles heated at 10 °C/min. The Brunauer-Emmett-Teller (BET) surface area was measured by N 2 physisorption at 77K with Micromeritics 3Flex. Material compositions were analyzed via Ion Chromatography (IC, ThermoFisher ICS 5000+). 2.5 Preparation of propellants Table 1 Formulation of solid propellants with Fe-CPs@AP nanoparticles employed as additional combustion modifier 20 62 3.6 14.4 3/4/5 In the standard formulation protocol, all raw materials underwent dehydration at 50°C for 120 minutes before processing to ensure moisture removal (Table 1). The composition included 41% ammonium perchlorate particles ranging from 210-354 μm in diameter, while finer particles measuring 125-147 μm constituted 21%. For formulations containing Fe-CPs@AP, the quantity of ammonium perchlorate in the combustion catalyst was proportionally reduced to maintain the overall 62% oxidizer content. Initial mixing involved combining aluminum powder, ammonium perchlorate, HTPB, MAPO, DOS, and functional modifiers through 60 minutes of mechanical blending prior to the addition of TDI. The composite was subjected to continuous agitation for 30 minutes to achieve homogeneity before being transferred to curing molds. The propellant slurry was cured at 50 ± 0.5°C for 168 hours. After that, it was cooled to room temperature and stored in a desiccator before measurement. All specimens were maintained under identical processing parameters including blending temperature, duration, and vacuum intensity during preparation. 2.6 Study on Combustion Characteristics Combustion performance evaluation was conducted in a transparent pressure chamber fitted with observation ports (Fig. 1). Internal pressure conditions were tracked using a PT301CS pressure sensor linked to a digital data recorder. Ignition sequences were triggered by activating an ignition enhancer at the specimen’s upper extremity. Test pressures spanned 3.0-9.0 MPa, with nitrogen serving as the pressurizing medium. The combustion flame was captured using a high-speed camera (Revealer M230C) to observe the flame structure and determine the burning rates based on the changes in the burning surface position over time. The timing initiated when the top surface of the propellant strip was fully consumed by combustion and terminated when the combustion process reached completion. The pixel position of the lowest point of the burning surface within a frame was designated as the burning surface position. Combustion velocity calculations followed the established relationship: ……….(1) Here, r p represented the combustion velocity, mm/s; l was the height of a single pixel, which was calculated by dividing the height of the sample by the number of pixels in the initial frame; f was the frame rate; X 1 and X 2 denoted the positions of combustion surface in the two frames; and N was the number of frames between these two frames. For experimental validation, each data point reflecting combustion rate precision was obtained through triplicate specimen averaging. Pressure exponent analysis utilized the Saint-Robert formulation r p = a * p n , where ’ a ’ represented the burning rate coefficient. Fig.1. Visual high pressure combustion test system 2.7 Computation Details The density functional theory (DFT) calculations were performed by implementing Vienna Ab initio Simulation Package (VASP) [27–30] . The exchange-correlation functional were treated within the generalized gradient approximation (GGA) using the Perdew-Burke-Ernzerhof (PBE) parametrization [31–33] for all calculations. Hubbard correction\(U_{\text{eff}}=5.3\ eV\) was applied to the GGA functionals for Fe atoms. Models for AP-Fe 3 O 4 were presented in Fig. 14. Here, the structure crystallizing in the ” Fd-3m ” space group was utilized for the bulk Fe 3 O 4 , and the typical (001) crystallographic surface was cleaved. During structural optimization, the two layers closest to the AP molecule were allowed to relax, while the remaining bottom layers were fixed. The structural relaxations terminated normally with residual forces that were not larger than 5×10 -2 eV/Å, while energy difference between successive self-consistent field (SCF) calculation steps were less than 1×10 -5 eV. The visualization for structure and charge density distributions were carried by VESTA software [34] . The bader charge analysis [35] was performed to quantity the charge density distributions. Results and Discussion 3.1 Characterization of Fe-CPs@AP A range of analytical methods, such as XPS and FTIR, were utilized to investigate the functionalized surfaces formed by Fe-CPs and Fe-CPs@AP energetic composites. Our research group has previously carried out a thorough and in-depth analysis of the Fe-CPs powder (Fig. 2). The XRD analysis indicated that the Fe-CPs powder consisted of C 10 H 10 FeN 8 O 6 (PDF#1511774), 4Fe(OH) 3 ·H 2 O (PDF#461436), and 2-methylimidazole (PDF#361686). Here, 2-methylimidazole was used as a raw material [26] . Fig.2. The analysis of XRD patterns from Fe-CPs The X-ray diffraction analysis of Fe-CPs@AP and Fe-CPs/AP composites confirmed effective deposition of ultrafine AP layers on Fe-CPs surfaces (Fig. 3). Sharp diffraction signals observed in Fe-CPs samples revealed localized crystalline ordering and nanoscale particle dimensions, while broadened weak reflections suggested predominant amorphous characteristics, consistent with earlier findings [36] . Characteristic AP diffraction angles at 15.5°, 19.6°, 22.9°, 24.1°, 24.9°, 30.3°, and 34.7° remained unmodified in Fe-CPs@AP specimens, confirming structural preservation of AP crystallites during coating processes. Conversely, Fe-CPs/AP displayed distinctive peaks at 13.8°, 17.7°, and 21.9° corresponding to pristine Fe-CPs material. Comparative analysis revealed that both composite materials maintained matching diffraction profiles with pure AP components, demonstrating successful integration through distinct surface treatment methods. These crystallographic observations collectively verify that neither preparation technique induced phase transformations in the AP crystalline lattice. Fig.3. XRD patterns from Fe-CPs@AP and Fe-CPs/AP The microstructure of the uncoated and coated powders was characterized using SEM (Fig. 4a and Fig. 5a). Unmodified particles displayed angular, fragmented morphology with size heterogeneity and surface porosity. Variations in particle density arose from differences in synthesis parameters and ligand-metal coordination dynamics. Post-coating analysis revealed Fe-CPs adopting geometric polyhedral configurations containing uniformly dispersed AP nanoparticles both externally and internally, with Fe5B-CPs@AP demonstrating approximate dimensions of 2 μm. EDAX images were utilized to verify the chemical composition and purity of the Fe-CPs (Fig. 4b). The results showed a homogeneous distribution of Fe, N, and O in the Fe-CPs, thus validating its synthesis. Subsequent EDAX evaluation of coated composites (Fig. 5b) illustrated consistent spatial distribution patterns for Fe, N, O, and chlorine elements, confirming material purity. This experimental evidence confirm the solvent-antisolvent methodology’s effectiveness in fabricating Fe-CPs@AP composite materials. (b) Fig.4. SEM and EDAX images of Fe-CPs The porous structure of Fe-CPs was characterized via N₂ adsorption/desorption. Prior to measurement, the samples were heated to 80 °C under vacuum for 12 h to remove adsorbed solvents. Figure S.1 displayed the obtained nitrogen sorption isotherms and pore size distribution profiles measured at 77 K. Previous studies by the research team [26] revealed that Fe-CPs possessed mesoporous characteristics with Type IV adsorption behavior. Surface area analysis demonstrated a substantial increase from 1.9718 m²/g for bare Fe-CPs to 43.4612 m²/g for the modified Fe-CPs@AP composite, representing a 22-fold enhancement. Pore dimension analysis showed a reduction from 3.44 nm in uncoated samples to 2.89 nm after AP modification. These alterations confirm AP’s effective interaction with Fe-CPs surfaces, which optimized active site accessibility and facilitated improved interfacial contact between catalytic centers and AP crystalline structures. FTIR analysis was employed to investigate the chemical structures and key functional groups of Fe-CPs, Fe-CPs@AP, and Fe-CPs/AP (Fig. 6). The Fe-CPs spectrum exhibited distinct absorption bands at 666 cm⁻¹ and 749 cm⁻¹, originating from Fe-O and Fe-N vibrational modes. In the spectra of Fe-CPs/AP and Fe-CPs@AP, the strong peaks at 616 cm⁻¹ and 653 cm⁻¹ as well as 626 cm⁻¹ and 667 cm⁻¹, were identified as characteristic Fe-O and Fe-N stretching modes [37] . Spectral features at 1079 cm⁻¹ (ClO₄⁻ stretching) and 1403 cm⁻¹ (NH₄⁺ bending) [38] confirmed the preservation of AP’s structural integrity post-encapsulation. The characteristic peaks at 3127 cm⁻¹ for Fe-CPs, 3275 cm⁻¹ for Fe-CPs/AP and Fe-CPs@AP were the -CH₃ stretching vibrations on the imidazole ring. The N-H bond peaks on the imidazole ring were at 1567 cm⁻¹ for Fe-CPs, 1562 cm⁻¹ for Fe-CPs/AP, and 1539 cm⁻¹ for Fe-CPs@AP. These spectral characteristics demonstrate the maintained structural framework of Fe-CPs within the composite materials. (b) Fig.5. SEM and EDAX images of Fe-CPs@AP Fig.6. FTIR spectra of Fe-CPs, Fe-CPs@AP and Fe-CPs/AP The XPS analysis of Fe-CPs@AP composites (Figs. 7 and S.2) revealed distinct Fe 2p 3/2 and Fe 2p 1/2 signals at 710.09 eV and 723.36 eV, corresponding to Fe²⁺ species [39] . Characteristic satellite peaks further confirmed both valence states, with Fe²⁺ showing signals at 712.36 eV/725.97 eV and Fe³⁺ exhibiting features at 718.62 eV/732.01 eV. The O 1s and N 1s spectra displayed prominent peaks at 529.67 eV and 398.74 eV, respectively, verifying the formation of Fe-O and Fe-N coordination bonds [40,41] . Distinct Cl 2p signals observed at 207.25 eV and 208.92 eV provided evidence for ClO₄⁻ incorporation within the composite structure [42] . Comparative analysis with the previously synthesized Fe-CPs nanoparticles we made showed XPS profiles (Fig. S.3) that closely matched those observed in Fe-CPs@AP particles. IC measurements (Fig. S.4) quantified the chloride ion content at 0.8%, corresponding to 2.6% ammonium perchlorate content and confirming complete surface coverage of Fe-CPs@AP by AP components. The dynamic composites maintain their unique morphological features, intricate structural designs, and abundant pore structures while simultaneously demonstrating a considerable surface area. This characteristic proves to be advantageous by broadening the interfacial contact with AP particles, enhancing the availability of active sites, and boosting catalytic performance. These findings collectively highlight Fe-CPs@AP particles as superior catalytic materials for enhancing the combustion rate. 3.2 Thermal decomposition analysis of Fe-CPs@AP The choice of catalyst materials for solid propellant combustion is critically reliant on thermal stability characteristics. TG-DSC analysis was employed to examine the thermal decomposition behavior of AP and Fe-CPs@AP nanocomposites. For pure AP, an endothermic phase transition from orthorhombic to cubic crystalline structure was observed at 245 ± 3℃ [43] , followed by two distinct decomposition stages. The initial exothermic event at 301 ± 5℃ represented low-temperature decomposition, while the subsequent high-temperature decomposition (HTD) occurred at 453 ± 5℃ [40] (Fig. S.5). During LTD, partial decomposition generated oxidizing agents (HClO 4 ) and fuel components (NH 3 ), with most ammonia molecules adhering to AP surfaces and inhibiting further breakdown. Complete decomposition occurred at HTD temperatures when NH 3 desorbs from the surface [44] . Fig.7. XPS spectra of Fe-CPs@AP Fig.8. TG-DSC curves of Fe-CPs@AP As depicted by the TG-DSC curves (Fig. 8), employing Fe-CPs as a catalyst, the weight-loss temperature range of AP was narrowed to 267 °C-314 °C. During the first weight-loss interval, the weight-loss rate of AP reached 29.5% at 340 °C. In contrast, in the initial weight-loss stage of Fe-CPs@AP, the weight-loss rate could reach 10.5% at 262 °C. Table 2 revealed that catalytic modification substantially enhanced thermal energy release, with composite materials demonstrating 2.3-fold greater heat emission compared with pure AP during high-temperature decomposition phases. Low-temperature decomposition stages also showed significant improvement, exhibiting 1.9 times higher energy release than unmodified AP. Thermal degradation completion analysis revealed pure AP achieved full gaseous conversion with 100% mass loss, while catalytic samples maintained residual solid components despite progressive heating. When Fe-based coordination polymers were embedded, the weight-loss rate decreased to 61.8%, accompanied by an increase in the residue rate. The incorporation of Fe-CPs brought about a notable alteration in the characteristic peaks of AP during its thermal decomposition process. The HTD peak temperature dropped from 430.1 °C to 296.7 °C, whereas the LTD peak temperature decreased from 303.1 °C to 282.2 °C. Compared to unmodified AP, the HTD phase demonstrated a notable 133.4°C advancement, with the LTD phase showing a 20.9°C temperature reduction. The temperature difference between the HTD and LTD peaks was merely 14.5 °C. This phenomenon can be ascribed to the adsorption of NH 3 generated during the low-temperature decomposition by Fe-CPs. Concurrently, the self-decomposition of Fe-based complexes destabilized NH 3 configurations, promoting conversion into nitrogen oxides (NO, NO₂, N₂O). These synergistic effects collectively enabled dramatic HTD peak suppression in AP, as evidenced by progressive thermal degradation patterns [23] . The catalytic mechanism primarily operated during AP’s high-temperature decomposition phase, mirroring conventional combustion catalyst functionality [2,45] . The TG-DSC analysis of Fe-CPs/AP revealed that an explosion occurred during the test (Fig. S.6). This was presumably mainly attributed to the non-uniform distribution of AP on the surface of Fe-CPs. Consequently, the heat release during the heating process was non-uniform, which subsequently induced the explosion. Comparative analysis revealed Fe-CPs incorporation significantly modified AP’s thermal decomposition behavior by shortening both LTD and HTD decomposition phases while lowering peak temperatures in both decomposition stages. The Fe-CPs@AP system leverages its nanoscale architecture to enhance catalytic efficiency through three primary factors: increased active site availability from expanded surface area, improved adsorption capacity for decomposition intermediates, and accelerated heat release at reduced temperatures. This structural configuration facilitates superior catalytic performance in AP decomposition compared to pure AP. Table 2 Maximum temperatures and net exothermicity of AP and Fe-CPs@AP Low High Low(-) High(-) AP 250.0 303.1 430.1 342.9 456.7 Fe-CPs@AP 243.6 282.2 296.7 647.0 1066.04 3.3 Research on the combustion rate with Fe-CPs@AP To delve deeper into the impact of Fe-CPs@AP energetic nanocomposites, Table 3 displayed a comparative analysis of combustion velocities in AP-HTPB propellants modified with distinct catalyst ratios. Table 3 Combustion rate of AP-HTPB propellants with Fe-CPs@AP with different ratios 3.0 MPa 5.0 MPa 7.0 MPa 9.0 MPa R 2 Blank 3.77 5.33 6.52 7.55 0.9979 0.633 3 wt% 5.65 8.01 9.71 10.51 0.9758 0.577 4 wt% 6.64 8.60 10.14 12.73 0.9727 0.571 5 wt% 6.30 7.93 9.35 11.27 0.9817 0.516 As depicted in Table 3 and Fig. 9, the unmodified propellant containing 62% oxidizer content displayed combustion velocities varying between 3.77 mm/s and 7.55 mm/s when tested under pressures of 3.0-9.0 MPa. When various ratios of combustion modifiers were incorporated, the modified propellants exhibited enhanced burning rates at different pressure levels. Specifically, formulations containing 3 wt% Fe-CPs@AP demonstrated combustion speeds of 5.65-10.51 mm/s, while those with 4 wt% Fe-CPs@AP achieved higher velocities of 6.64-12.73 mm/s within equivalent pressure parameters. The 5 wt% modified propellant exhibited combustion rates spanning 6.30-11.27 mm/s, surpassing the baseline propellant’s performance under identical conditions. Notably, these enhanced formulations displayed reduced pressure index values, indicating improved combustion stability with minimized sensitivity to chamber pressure variations. Notably, within the Fe-CPs@AP additive series, the 4 wt% formulation exhibited superior combustion acceleration effects. At respective pressures of 3.0, 7.0, and 9.0 MPa, this formulation enhanced burning velocities by 43%, 34%, and 41% compared to control samples. This performance optimization stems from achieving an ideal dispersion balance between Fe-CPs@AP and the propellant matrix, facilitating uniform catalyst distribution across the slurry surface. However, when the addition amount of Fe-CPs@AP reached 5 wt%, the combustion rate decreased. This might be attributed to the fact that the excessive doping of Fe-CPs hindered the release of reaction heat and could potentially result in excessive agglomeration of ultrafine AP particles. Therefore, the 4 wt% Fe-CPs@AP nanocomposite material exhibited the most remarkable performance in the combustion catalysis of the propellant. Fig. 10 visually presented the recorded images of the stable combustion process of the propellant under low and high pressure conditions and carried out an in-depth comparative analysis. When compared with the blank sample, the flame of the propellant containing the combustion catalyst was brighter. Furthermore, in comparison with the AP-HTPB propellant containing 4 wt% Fe-CPs@AP at 3.0 MPa, the flame of the AP-HTPB propellant at 9.0 MPa demonstrated more distinct red flame characteristics and a shorter duration, which was highly consistent with the above research results. Additionally, in a high-pressure environment, the flame structure of the composite propellant containing 4wt% Fe-CPs@AP was flatter. Fig.9. Comparison of combustion rates of pristine AP-HTPB propellants employed with Fe-CPs@AP at various ratios (b) Fig.10. The combustion process of AP-HTPB solid propellant in the presence and absence of a catalyst (a) Blank (b) 4wt% Fe-CPs@AP 3.4 Characteristics of the combustion residue The combustion residue of the solid propellant specimen was gathered for XRD, SEM, and EDAX analysis. As depicted in Fig. 11, the composition of the residue differed from that of Fe-CPs@AP nanoparticles. By comparing PDF#890691 and PDF#892468, the results revealed complex crystallization patterns, encompassing cubic Fe 3 O 4 and FeO phases. Evidently, the degradation, oxidation, and transformation of Fe-CPs@AP nanoparticles gave rise to the formation of Fe 3 O 4 , FeO, and their derivatives. Notably, nanoscale Fe 3 O 4 particles demonstrated significant research value due to their versatile magnetic characteristics. This material typically manifested four crystalline variants (α-Fe 2 O 3 , β-Fe 2 O 3 , γ-Fe 2 O 3 , and ε-Fe 2 O 3 ), each displaying unique magnetic behaviors as documented in reference [46] . The Fe element was found to be uniformly distributed on the surface of the combustion residue, indicating that the metal oxides derived from Fe-CPs catalyze the combustion in a more uniform way (Fig. 12). Fig.11. Powder X-ray patterns from combustion residue Fig.12. SEM and EDAX images of combustion residue 3.5 Catalytic mechanism The thermal degradation process of ammonium perchlorate constitutes an intricate multi-stage reaction system, with comprehensive understanding of its decomposition pathways still requiring further investigation. Based on the commonly accepted proton transfer theory [47] , both the low-temperature decomposition and high-temperature decomposition stages involve the decomposition of AP into NH 3 and HClO 4 . Subsequent redox processes between these decomposition products yield volatile substances including HCl and H 2 O. Intermediate products, including O₂, NO, and N₂O, are produced when ClO₃ accepts electrons to generate ClO 3 ⁻. This ClO 3 ⁻ then participates in a typical solid-gas two-phase reaction with NH₃, as elaborated in Equations (1)-(5) [48] . NH 4 ClO 4 → NH 4 + + ClO 4 - ↔ NH 3 + HClO 4 (1) NH 4 + + e - → NH 3 + H (hydrogen atom) (2) ClO 4 - + H → HClO 4 (3) HClO 4 + H → ClO 3 + H 2 O (4) ClO 3 + e - → ClO 3 - (5) O 2 + e - → O 2 - (6) NH 3 +O 2 - → N 2 O + NO 2 + H 2 O + e - (7) The Fe-CPs@AP energetic composites possess a large specific surface area, pore volume, and numerous catalytic sites. These structural advantages allow the materials to effectively capture and concentrate NH₃ and HClO₄ while spatially confining their reactive environment. When exposed to gaseous byproducts, the coordination polymers undergo structural reorganization into corresponding metal oxides [49] . These oxide derivatives demonstrate semiconductor characteristics, particularly Fe species with partially occupied 3d-electron orbitals. Their unique hole-dominated quasi-conductive nature [50] enables catalytic enhancement of ammonium perchlorate decomposition through two crucial mechanisms: facilitating proton migration between ClO₄⁻ and NH₄⁺ ions, and accelerating superoxide ion (O₂⁻) generation kinetics. This dual catalytic effect markedly promotes ammonia conversion into NOₓ species and water molecules as described in Equations (6)-(7). In light of the aboved-mentioned results, the existence of Fe-CPs@AP energetic composites exerts a profound influence on the thermal reaction transitions of AP. This catalytic activity becomes particularly noticeable within the HTD zone, characterized by unique polyhedral structures. Such geometric configurations significantly increase accessible catalytic surfaces while promoting electron transport efficiency, primarily due to Fe-containing components. Observable shifts in thermal emission peaks suggest intensified electronic interactions that promote AP’s thermal breakdown. These findings highlight the exceptional performance of Fe-CPs@AP as a burning rate catalyst. Fig.13. Mechanistic Schematic of AP’s decomposition processes catalyzed by Fe-CPs@AP 3.6 DFT calculation To delve deeper into the influence of metal oxides on AP’s thermal decomposition process, density functional theory (DFT) simulations were employed to clarify the electron transfer dynamics regulating this process on Fe₃O₄ surfaces. Fig. 14 (a) illustrated the total energies of the initial, intermediate, and final states throughout the decomposition process. The initial state featured the adsorbed reactants NH 4 + and ClO 4 - , while the final state comprised the products NH 3 and HClO 4 , with a DFT total energy of -0.22 eV. Under the catalytic influence of the Fe₃O₄ surface, the reaction proceeded via a key intermediate state. Here, the NH 4 + cation underwent deprotonation, releasing an H⁺ ion that bonds to a surface O atom. Charge analysis, quantified by Bader charges and visualized in Fig.14 (b), revealed significant redistribution during this proton transfer. The bonded H atom gained a charge of -0.62 e, while the surface O atom gained +0.39 e. Concurrently, the intermediate products ClO₄ ⁻ and NH₃ adsorbed onto surface Fe atoms. Adsorption induced further charge transfer, with an O atom in ClO₄⁻ gaining +0.46 e, the N atom in NH₃ gaining +0.14 e, and neighboring Fe atoms collectively gaining approximately -0.3 e. This adsorption stabilized the intermediate configuration, lowering its DFT total energy by 2.42 eV relative to the initial state. The significant stabilization energy (-2.42 eV) and observed charge redistributions suggested that the thermal decomposition of ammonium perchlorate was expedited by multiple electron transfer processes taking place at the interface between AP and the Fe₃O₄ surface. Fig.14. (a) Initial-, intermediate- and final-state models of the AP-Fe 3 O 4 are presented. The DFT total energies are referenced to the initial state energy through setting\(E_{\text{initial}}=0\ \text{eV}\) . (b) The charge differences for the AP-Fe 3 O 4 model at the intermediate state are presented with an isosurface level of \(0.004\ \text{a.\ u.}\) The bader charge differences are labeled for several atoms. 4. Conclusions To systematically explore the catalytic effects on ammonium perchlorate’s thermal decomposition, a solvent-nonsolvent approach for fabricating Fe-CPs@AP hybrid materials has been utilized. The synthesized catalysts exhibit remarkable polyhedral architecture with expansive surface area, exceptional thermal resistance, and robust electron transport capabilities derived from Fe-based structural frameworks and metallic active components. Such structural advantages contribute to a marked reduction in AP’s high-temperature decomposition threshold while substantially boosting its exothermic energy output. When incorporated at 4 % mass fraction in solid propellants, Fe-CPs@AP demonstrates superior combustion characteristics including reduced pressure dependence coefficients, effective suppression of AP nanoparticle coalescence, optimized catalytic performance with minimized catalyst migration. The mechanistic study reveals that Fe-based functional frameworks and active metal centers effectively function as electron transfer mediators, enhancing charge exchange efficiency between ClO 4 - and NH 4 + ions during low-temperature decomposition phases. Throughout high-temperature decomposition stages, Fe-CPs@AP’s abundant active sites enable in situ formation of metal oxide species. This catalytic transformation significantly enhances the adsorption of oxygen-containing species during the thermal degradation process of AP and facilitates accelerated electron transfer. These results are in good agreement with the density functional theory simulations. These characteristics position Fe-CPs@AP as a promising high-performance catalyst with reduced sensitivity for AP-based composite propellants requiring rapid combustion rates. Supporting information Fig.S.1. N 2 adsorption/desorption isotherms and pore-size distributions of Fe-CPs and Fe-CPs@AP. Fig.S.2. The full spectra of Fe-CPs@AP. Fig.S.3. XPS spectra of Fe-CPs. Fig.S.4. IC results of Fe-CPs@AP. Fig.S.5. TG-DSC curves of AP. Fig.S.6. TG-DSC curves of Fe-CPs/AP Acknowledgement This work was supported by the National Natural Science Foundation of China, Joint Fund Project [grant numbers U22B20138]. References 1. Chen, F.; Xuan, C.; Lu, Q.; Xiao, L.; Yang, J.; Hu, Y.; Zhang, G.; Wang, Y.; Zhao, F.; Hao, G.; Jiang, W. A review on the high energy oxidizer ammonium dinitramide: its synthesis, thermal decomposition, hygroscopicity, and application in energetic materials. Def. Technol. 2023 , 19 , 163－195. 2. Yadav, N.; Srivastava, P.K.; Varma, M. 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Keywords adjustable decomposition of ap ap-htpb propellant burning catalyst fe-based functional coordination polymers Authors Affiliations Yan Zhao National University of Defense Technology View all articles by this author Bian Li National University of Defense Technology View all articles by this author Guixi Liu Power Machinery Institute of Inner Mongolia View all articles by this author Tao Zhang Power Machinery Institute of Inner Mongolia View all articles by this author Xiaoyu Lv Power Machinery Institute of Inner Mongolia View all articles by this author Chaohui Guo Power Machinery Institute of Inner Mongolia View all articles by this author Jiexin Weng Power Machinery Institute of Inner Mongolia View all articles by this author Zhou Xing 0000-0002-9980-1937 [email protected] National University of Defense Technology View all articles by this author Shuo Liu Huaqiao University - Xiamen Campus View all articles by this author Zhongyun Ma Xiangtan University School of Chemistry View all articles by this author Metrics & Citations Metrics Article Usage 212 views 49 downloads .FvxKWukQNSOunydq8rnd { width: 100px; } Citations Download citation Yan Zhao, Bian Li, Guixi Liu, et al. 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