Fabrication of three-dimensional TKX-50 network-like nanostructures by liquid nitrogen-assisted spray freeze-drying method

Xiong, Chunhua; Shang, Yiping; Meng, Ke-Juan; Yue, Guodong; Yang, Liyuan; Liu, Yang; Deng, Peng; Hu, Lishuang

doi:10.1080/07370652.2019.1585491

Cited by 24 publications

(5 citation statements)

References 37 publications

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“…As shown from Figure 4, the characteristic peaks of TKX-50 appeared at 2θ = 15.1°, 15.3°, 25.2°, 26.6°, 27.9°, and 29.7°, which corresponded to the (020), ( 011), (12-1), ( 121), (130), and (040) planes of TKX-50, respectively [34]. The peak shape and peak position of TKX-50(ss) remained basically unchanged, indicating that no crystal phase transformation occurred during spray drying process.…”

Section: Composition and Structuresmentioning

confidence: 96%

Preparation and characterization of superfine spherical TKX‐50 with a hollow structure by spray drying

Wang

Jiang

Zong

et al. 2023

Propellants Explo Pyrotec

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Micro/nano energetic materials with regular morphologies exhibit high energy release efficiency, superior charge performance, and low mechanical sensitivity. Exploring dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50) with spherical microstructures and excellent comprehensive properties is of great significance for potential applications. In this work, a kind of superfine spherical TKX-50 was fabricated by spray drying method. The as-prepared TKX-50 had a narrow particle size distribution with d 50 = 3.14 μm, high sphericity of 0.944 with hollow structure and bulk density of 1.851 g/cm 3 . And its formation mechanism was proposed. The results of XRD and FT-IR demonstrated that spray drying would not change the crystal structure of TKX-50. TG-DSC results showed that the initial decomposition and the peak temperature of superfine spherical TKX-50 was about 10 °C lower than raw TKX-50, and the apparent activation energy was 4.584 kJ • mol À 1 lower than raw TKX-50, due to the dramatic change in morphology. TG-DSC-FTIR-MS provided a new understanding of decomposition process of TKX-50, and the results illustrated that the main gas products were N 2 , H 2 O, N 2 O, NH 3 , NO, NH 2 , CO 2 , and HCN. Superfine spherical TKX-50 underwent similar decomposition path as raw TKX-50 but stood out in its larger occupation of the first decomposition which meant a more complete decomposition and its faster rate of the whole decomposition process. More importantly, the impact sensitivity (H 50 ) increased from 50.1 cm to 70.8 cm, and the friction sensitivity (P) decreased from 24 % to 0 %, showing improved safety performance.

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Section: Composition and Structuresmentioning

confidence: 96%

Preparation and characterization of superfine spherical TKX‐50 with a hollow structure by spray drying

Wang

Jiang

Zong

et al. 2023

Propellants Explo Pyrotec

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“…Among the various 3D rGO synthesis methods, such as chemical reduction process, [47][48][49] electrochemical process, 50,51 spray-freezing method was selected due to its 3D radially opened structural advantages. [52][53][54] Also, the spray-freezing method can directly utilize the aqueous GO solution and that process is safe and facile. sprGO is fabricated through lowtemperature spray-freezing method.…”

Section: Introductionmentioning

confidence: 99%

“…To compensate for this drawback, sprGO, which has a 3D morphology with graphene sheets, is suggested here. Among the various 3D rGO synthesis methods, such as chemical reduction process, 47‐49 electrochemical process, 50,51 spray‐freezing method was selected due to its 3D radially opened structural advantages 52‐54 . Also, the spray‐freezing method can directly utilize the aqueous GO solution and that process is safe and facile.…”

Section: Introductionmentioning

confidence: 99%

Maximizing the enzyme immobilization of enzymatic glucose biofuel cells through hierarchically structured reduced graphene oxide

Lee

Hyun

Park

et al. 2021

Intl J of Energy Research

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The number of immobilized glucose oxidase (GOx) molecules is considerably increased by the structural modification of reduced graphene oxide (rGO), and the performance of enzymatic biofuel cells (EBFCs) is positively affected by the modification process. To do this, new rGO with three-dimensional open porous structure is formed by spray freeze drying method (sprGO), while tetrathiafulvalene (TTF) as mediator, and GOx are sequentially immobilized onto sprGO. To improve the loading amount of catalyst, rGO structure is modified to open porous sprGO structure possessing numerous anchoring sites, after which gelatin film crosslinked by glutaraldehyde is fabricated onto sprGO to prevent any losses of other components (sprGO/[TTF-GOx]/crosslinked-gelatin). Specific surface area and charge transfer resistance of sprGO are quantitatively measured, and the actual amount of immobilized GOx and the performance of EBFC using this catalyst are electrochemically examined. With this, it is found that the amount of GOx immobilized in sprGO/[TTF-GOx]/

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“…In recent years, it has been an important research direction in the field of explosives to seek a kind of energetic material with high power and insensitive nature. As a typical tetrazole derivative, nitrogen rich high energy density compound TKX-50 contains a large amount of N–N bonds, C–N bonds, and a large ring tension compared with traditional nitramine and nitro energetic materials. , A large number of literatures indicate that − the detonation velocity of TKX-50 (9698.0 m s –1 ) is higher than that of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20, 9455.0 m s –1 ) and 1,3,5-trinitro-1,3,5-triazinane (RDX, 8983.0 m s –1 ). Its detonation pressure (42.4 GPa) is also higher than that of 2,4,6-trinitrobenzene (TNT, 23.5 GPa), RDX (38.0 GPa) and 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (β-HMX, 41.5 GPa).…”

Section: Introductionmentioning

confidence: 99%

Thermal Decomposition Characteristics and Thermal Safety of Dihydroxylammonium 5,5′-Bistetrazole-1,1′-diolate Based on Microcalorimetric Experiment and Decoupling Method

Tan

Cao

et al. 2020

J. Phys. Chem. C

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A microcalorimeter (C600) was used to conduct dynamic heating experiments on dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate (TKX-50), and the results were compared with those of differential scanning calorimetry (DSC). The effect of mass scale on the thermal decomposition characteristics of TKX-50 was also analyzed. The thermal decomposition curves were decoupled by mathematical method, and the kinetic parameters of each step were obtained. The thermal decomposition characteristics of TKX-50 were further analyzed by thermal history and isothermal experiment, and the thermal safety parameters were calculated by thermal analysis software (AKTS). The decomposition temperature and decomposition enthalpy of TKX-50 in the microcalorimetric experiment were higher than the corresponding parameters in the DSC experiment, and the apparent activation energy was lower than the one in the DSC experiment. When the times to maximum rate under adiabatic conditions were 2.0, 4.0, 8.0, and 24.0 h, the corresponding temperatures were 198.5, 189.6, 181.0, and 168.0 °C, respectively. After decoupling, the range of exothermic peak temperature and decomposition enthalpy of the first and second stages of TKX-50 were 226.9−245.3 and 276.3−295.7 °C and 1300.7 and 727.7 J g −1 , respectively, and the apparent activation energy of the second stage was higher than that of the first stage. The thermal history reduced the decomposition temperature and the apparent activation energy of TKX-50, the safety was reduced, and this had a great influence on the thermal decomposition kinetics of TKX-50. Thermal history and isothermal experiment showed that the first stage decomposition reaction of TKX-50 has autocatalytic properties. Therefore, it should be prevented from being placed in an adiabatic environment, and it is necessary to avoid the storage of a large mass of TKX-50 and keep the heat source off the storage location in the process of industrial production and storage, so as to prevent the formation of adiabatic environments and thermal history in the interior and further reduce the risk of explosion in TKX-50.

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Fabrication of three-dimensional TKX-50 network-like nanostructures by liquid nitrogen-assisted spray freeze-drying method

Cited by 24 publications

References 37 publications

Preparation and characterization of superfine spherical TKX‐50 with a hollow structure by spray drying

Preparation and characterization of superfine spherical TKX‐50 with a hollow structure by spray drying

Maximizing the enzyme immobilization of enzymatic glucose biofuel cells through hierarchically structured reduced graphene oxide

Thermal Decomposition Characteristics and Thermal Safety of Dihydroxylammonium 5,5′-Bistetrazole-1,1′-diolate Based on Microcalorimetric Experiment and Decoupling Method

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