Fluorodinitroethyl Ortho-carbonate and -formate as Potential High Energy Dense Oxidizers

2014 ◽  
Vol 69 (1) ◽  
pp. 8-16 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Richard Moll ◽  
Sebastian F. Rest ◽  
Muhamed Sućeska
Keyword(s):  
Electrostatic Discharge ◽  
High Energy ◽  
Small Scale ◽  
Detonation Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dsc Measurements ◽  
Multinuclear Nmr Spectroscopy ◽  
Ray Density ◽  
Ir And Raman

Tetrakis(2-fluoro-2,2-dinitroethyl) ortho-carbonate (1) and tris(2-fluoro-2,2-dinitroethyl) orthoformate (2) were synthesized by the reaction of carbon tetrachloride, respectively chloroform, with 2-fluoro-2,2-dinitroethanol and catalytic amounts of anhydrous iron(III) chloride. The compounds were characterized by single-crystal X-ray diffraction, vibrational spectroscopy (IR and Raman), multinuclear NMR spectroscopy, elemental analysis, and multi-temperature DSC measurements. The suitability of the compounds as potential oxidizers in energetic formulations has been investigated and discussed. The heats of formation of the products were determined experimentally using bomb calorimetric methods. With this value and the experimental (X-ray) density, several detonation parameters such as the detonation pressure, velocity, energy, and temperature were computed using the EXPLO5 code. The sensitivity towards impact, friction and electrostatic discharge was tested using the BAM drop hammer, a friction tester and a small-scale electrostatic discharge device.

1-Amino-3-nitroguanidine (ANQ) in High-performance Ionic Energetic Materials

2012 ◽  
Vol 67 (6) ◽  
pp. 573-588 ◽  
Author(s):  
Niko Fischer ◽  
Thomas M. Klapötke ◽  
Jörg Stierstorfer
Keyword(s):  
Nitric Acid ◽  
Energetic Materials ◽  
Electrical Discharge ◽  
High Performance ◽  
Small Scale ◽  
Detonation Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dsc Measurements ◽  
Explosive Performance

1-Amino-3-nitroguanidine (ANQ, 2) was synthesized via hydrazinolysis of nitroguanidine (1). An appropriate Lewis structure of ANQ is drawn based on VB calculations. Due to its basicity, it can be protonated by strong mineral acids or acidic heterocycles. In order to synthesize new energetic materials the nitrate (3) and perchlorate (4) salts of 1-amino-3-nitroguanidine were synthesized by protonation of 2 with 40% nitric acid and 60% perchloric acid, respectively. 5-Nitrimino-1,4H-tetrazole obtained by reacting 5-amino-1H-tetrazole with 100% HNO3 was used to synthesize the nitriminotetrazolate salt 5. Furthermore, the dinitramide salt 6 of 1-amino-3-nitroguanidine was synthesized by metathesis reaction of silver dinitramide and 1-amino-3-nitroguanidinium chloride. The dinitroguanidinate salt 7 was synthesized by protonation of 2 with 1,3-dinitroguanidine, which was prepared from nitroguanidine in anhydrous nitric acid/N2O5. All compounds were fully characterized by singlecrystal X-ray diffraction, vibrational spectroscopy (IR and Raman), multinuclear NMR spectroscopy, mass spectrometry, elemental analysis, and DSC measurements. The heats of formation of 2 - 7 were calculated using the atomization method based on CBS-4M enthalpies. With these values and the experimental (X-ray) densities several detonation parameters such as the detonation pressure, velocity, energy, and temperature were computed using the EXPLO5 code. In addition, the sensitivities towards impact, friction and electrical discharge were tested using the BAM drophammer, friction tester as well as a small-scale electrical discharge device. A Koenen test with 1-amino-3-nitroguanidinium nitrate (3) was carried out in order to evaluate its explosive performance and shipping classification.

Characterizations of Synthetic 8mol% YSZ with Comparison to 3mol %YSZ for HT-SOFC

2020 ◽  
Vol 38 (4A) ◽  
pp. 491-500
Author(s):  
Abeer F. Al-Attar ◽  
Saad B. H. Farid ◽  
Fadhil A. Hashim
Keyword(s):  
Ionic Conductivity ◽  
Electrochemical Impedance ◽  
Structural Information ◽  
Impedance Analysis ◽  
High Energy ◽  
Yttria Stabilized Zirconia ◽  
X Ray Diffraction ◽  
Stabilized Zirconia ◽  
Powder Morphology ◽  
X Ray

In this work, Yttria (Y2O3) was successfully doped into tetragonal 3mol% yttria stabilized Zirconia (3YSZ) by high energy-mechanical milling to synthesize 8mol% yttria stabilized Zirconia (8YSZ) used as an electrolyte for high temperature solid oxide fuel cells (HT-SOFC). This work aims to evaluate the densification and ionic conductivity of the sintered electrolytes at 1650°C. The bulk density was measured according to ASTM C373-17. The powder morphology and the microstructure of the sintered electrolytes were analyzed via Field Emission Scanning Electron Microscopy (FESEM). The chemical analysis was obtained with Energy-dispersive X-ray spectroscopy (EDS). Also, X-ray diffraction (XRD) was used to obtain structural information of the starting materials and the sintered electrolytes. The ionic conductivity was obtained through electrochemical impedance spectroscopy (EIS) in the air as a function of temperatures at a frequency range of 100(mHz)-100(kHz). It is found that the 3YSZ has a higher density than the 8YSZ. The impedance analysis showed that the ionic conductivity of the prepared 8YSZ at 800°C is0.906 (S.cm) and it was 0.214(S.cm) of the 3YSZ. Besides, 8YSZ has a lower activation energy 0.774(eV) than that of the 3YSZ 0.901(eV). Thus, the prepared 8YSZ can be nominated as an electrolyte for the HT-SOFC.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

scholarly journals In-Situ High-Energy X-ray Diffraction Study of Austenite Decomposition During Rapid Cooling and Isothermal Holding in Two HSLA Steels

2021 ◽  
Vol 52 (5) ◽  
pp. 1812-1825
Author(s):  
Sen Lin ◽  
Ulrika Borggren ◽  
Andreas Stark ◽  
Annika Borgenstam ◽  
Wangzhong Mu ◽  
...  
Keyword(s):  
Isothermal Holding ◽  
Weight Percent ◽  
High Energy ◽  
Decomposition Kinetics ◽  
Bainitic Transformation ◽  
Austenite Decomposition ◽  
X Ray Diffraction ◽  
Rapid Cooling ◽  
X Ray

AbstractIn-situ high-energy X-ray diffraction experiments with high temporal resolution during rapid cooling (280 °C s−1) and isothermal heat treatments (at 450 °C, 500 °C, and 550 °C for 30 minutes) were performed to study austenite decomposition in two commercial high-strength low-alloy steels. The rapid phase transformations occurring in these types of steels are investigated for the first time in-situ, aiding a detailed analysis of the austenite decomposition kinetics. For the low hardenability steel with main composition Fe-0.08C-1.7Mn-0.403Si-0.303Cr in weight percent, austenite decomposition to polygonal ferrite and bainite occurs already during the initial cooling. However, for the high hardenability steel with main composition Fe-0.08C-1.79Mn-0.182Si-0.757Cr-0.094Mo in weight percent, the austenite decomposition kinetics is retarded, chiefly by the Mo addition, and therefore mainly bainitic transformation occurs during isothermal holding; the bainitic transformation rate at the isothermal holding is clearly enhanced by lowered temperature from 550 °C to 500 °C and 450 °C. During prolonged isothermal holding, carbide formation leads to decreased austenite carbon content and promotes continued bainitic ferrite formation. Moreover, at prolonged isothermal holding at higher temperatures some degenerate pearlite form.

Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.

scholarly journals Spatially Resolved Forming Mechanisms Detection in Single Point Incremental Forming Using Synchrotron Based Texture Analysis

2021 ◽  
Author(s):  
Mateus Dobecki ◽  
Alexander Poeche ◽  
Walter Reimers
Keyword(s):  
Texture Analysis ◽  
Incremental Forming ◽  
Single Point ◽  
High Energy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Forming Mechanism ◽  
Spatially Resolved ◽  
Step Down ◽  
Stress States

AbstractDespite the ongoing success of understanding the deformation states in sheets manufactured by single-point incremental forming (SPIF), the unawareness of the spatially resolved influence of the forming mechanisms on the residual stress states of incrementally formed sheet metal parts impedes their application-optimized use. In this study, a well-founded experimental proof of the occurring forming mechanisms shear, bending and stretching is presented using spatially resolved, high-energy synchrotron x-ray diffraction-based texture analysis in transmission mode. The measuring method allows even near-surface areas to be examined without any impairment of microstructural influences due to tribological reactions. The depth-resolved texture evolution for different sets of forming parameters offers insights into the forming mechanisms acting in SPIF. Therefore, the forming mechanisms are triggered explicitly by adjusting the vertical step-down increment Δz for groove, plate and truncated cone geometries. The texture analysis reveals that the process parameters and the specimen geometries used lead to characteristic changes in the crystallites’ orientation distribution in the formed parts due to plastic deformation. These forming-induced reorientations of the crystallites could be assigned to the forming mechanisms by means of defined reference states. It was found that for groove, plate and truncated cone geometries, a decreasing magnitude of step-down increments leads to a more pronounced shear deformation, which causes an increasing work hardening especially at the tool contact area of the formed parts. Larger step-down increments, on the other hand, induce a greater bending deformation. The plastic deformation by bending leads to a complex stress field that involves alternating residual tensile stresses on the tool and residual compressive stresses on the tool-averted side incrementally formed sheets. The present study demonstrates the potential of high-energy synchrotron x-ray diffraction for the spatially resolved forming mechanism research in SPIF. Controlling the residual stress states by optimizing the process parameters necessitates knowledge of the fundamental forming mechanism action.

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