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1.
The parent material, ammonium permanganate, was carefully decomposed in air at 120°. The product, referred to as the starting material (SM), was then subjected to thermal treatment in air for 5 hr in the temperature range 150–1200°. Chemical analysis of SM indicated that the main decomposition product of NH4MnO4 was Mn2O3, together with MnO2, NH4NO3, H2O and O2. Mn3O4 started to form at 900°. The infrared spectra of various calcination products revealed the retention of NH 4 + in the lattice structure up to 300°, and reflected the presence of excess oxygen as coordinated O 2 . The TG, DTA and IRA results on SM supported the chemical analysis data. X-ray analysis was carried out for phase identification and to follow transformations and the formation of a solid solution between MnO2 and Mn2O3.
Zusammenfassung Die Muttersubstanz, Aramoniumpermanganat, wurde in Luft bei 120° vorsichtig zersetzt. Das dabei erhaltene Ausgangsmaterial (SM) wurde danach in Luft 5 Stunden im Temperaturbereich von 150–1200° thermisch behandelt. Die chemische Analyse von SM ergab, daß als Hauptprodukt der Zersetzung von NH4MnO4, Mn2O3 auftritt neben MnO2, NH4NO3, H2O und O2. Die Bildung von Mn3O4 beginnt bei 900°. Aus Infrarotspektren verschiedener Kalzinierungsprodukte ist ersichtlich, daß in der Gitterstruktur NH 4 + bis 300° zurückgehalten wird und überschüssiger Sauerstoff in Form von koordiniertem O2 vorliegt. Die Ergebnisse der TG-, DTA- und IRA-Untersuchungen von SM bestätigen Daten der chemischen Analyse. Mittels Röntgenanalyse wurden die Phasen identifiziert und der Verlauf der Phasenübergänge und der Bildung einer festen Lösung zwischen MnO2 und Mn2O3 verfolgt.

120°. , , 5 150–1200°. , , , , . 900° Mn3O4. 300° - O 2 . , . , .


Paper presented at the World Conference on Thermal Analysis, Madeira (Portugal), 1986.  相似文献   

2.
3.
Thermal decomposition of ammonium perchlorate   总被引:10,自引:0,他引:10  
This review represents an attempt to summarize literature data on thermal decomposition of ammonium perchlorate. The mechanism of thermal decomposition and various factors which influence on the thermal decomposition of ammonium perchlorate are discussed.  相似文献   

4.
The thermal decomposition of ammonium uranates precipitated from uranyl nitrate solution on the addition of aqueous ammonium hydroxide and hexamine under various conditions has been studied by means of thermogravimetry, differential thermal analysis, infrared spectroscopy and X-ray diffraction. Although all precipitates show the composition corresponding to UO3 · NH3 · H2O, the precipitates with hexamine give X-ray diffraction patterns designed as types I and II, in which type I is similar to the precipitates with ammonia. As a result, it is concluded that ammonium uranates thermally decompose to amorphous UO3 at about 400°, and transform to U3O8 via-UO3 and/or-UO3, latter being formed in the case of type II only.
Zusammenfassung Die thermische Zersetzung von unter verschiedenen Bedingungen durch wässrige Lösungen von Ammoniumhydroxid und Hexamin aus Uranylnitrat-Lösung gefällten Ammoniumuranaten wurde mittels TG, DTA, IR-Spektroskopie und Röntgendiffraktometrie untersucht. Obwohl die Zusammensetzung aller Niederschläge der Formel UO3 · NH3 · H2O entspricht, geben die mit Hexamin gefällten Niederschläge die als Typ I und II bezeichneten Röntgendiffraktogramme, von denen das des Typs I ähnlich dem der mit Ammoniak gefällten Niederschlage ist. Es wird festgestellt, daß Ammoniumuranate bei 400° thermisch zu amorphen UO3 zersetzt werden und sich über-UO3 und/oder-UO3—wobei beim Typ II nur das letztere gebildet wird — in U3O8 umwandeln.

, , - - , . @2 UO3 · NH3 · H2O, , - I II. . , 400° UO3 U3O8 -UO3 -UO3. II.
  相似文献   

5.
Ammonium metavanadate is subjected to thermal treatment in the range 180–550°C and structural and surface area changes are studied by X-ray diffraction and N2 adsorption. DTA and TGA show the existence of a large endotherm (260°C) possibly composed of several stages, and a much smaller one (340°C) which is responsible for evolution of the molecule of water associated with the V2O5 initially formed. Three exotherms also appear and explanations for their presence are given. The phases formed, as well as the specific surface areas, are determined for the products obtained in a vacuum and in the presence of water vapour, and changes in surface areas are related to the phase transformations and dehydration of the products formed during thermal treatment.  相似文献   

6.
7.
The thermal decomposition of ammonium ceryl(III) carbonate (ACeC) [NH4CeO(CO3)] was investigated by thermogravimetry, differential thermal analysis and X-ray diffraction. The results showed three endothermic stages of decomposition, each involving a loss in weight. The first stage, at 65.5 °C, is characteristic of the removal of adsorbed water, the second stage, at 214.8 °C, is associated with ammonia release, and the third stage, at 263.6 °C, relates to the removal of carbon dioxide.  相似文献   

8.
Thermal decomposition of tetraethyl ammonium tetrafluoroborate has been studied employing simultaneous techniques of TG–DTG–DSC—quadrupole mass spectrometric techniques in an inert atmosphere of pure Helium gas at a sample heating rate of 5 K min?1 employing a platinum crucible. The observed decomposition paths are the most commonly expected Hofmann elimination and substitution reactions paths.  相似文献   

9.
Isothermal decomposition of orthorhombic ammonium perchlorate (AP) has been studied as a function of concentration of the dopants, SO 4 2– and PO 4 3– . In either case, the rate of decomposition passes through a maximum as the dopant concentration increases. Activation energy of the decomposition process remains unaltered by doping. The results are interpreted in terms of electron transfer mechanism.
Zusammenfassung Die isotherme Zersetzung von orthorhombischen Ammoniumperchlorat (AP) wurde in Abhängigkeit von der Konzentration der Dopanten SO 4 2– und PO 4 3– untersucht. In jedem Falle geht die Geschwindigkeit der Zersetzung mit steigender Dopantenkonzentration durch ein Maximum. Die Aktivierungsenergie des Zersetzungsprozesses wird durch dopen nicht verändert. Die Ergebnisse werden auf einem Elektronentransfer-Mechanismus basierend interpretiert.

- - . . . .


The author is thankful to Dr. V. R. Pai Verneker of Indian Institute of Science, Bangalore, for stimulating discussions.  相似文献   

10.
Journal of Thermal Analysis and Calorimetry - Les anomalies que nous avons observées, dans le cas de l'oxydation de fils de nickel, peuvent s'interpréter en faisant appel à...  相似文献   

11.
The thermal decomposition of large single crystals of pure ammonium perchlorate and ammonium perchlorate doped with Ba2+ or SO2?4 ions has been investigated over the temperature range 220–290°C. Comparative studies were also made with compressed pellets of the pure powder and with small single crystals containing macroscopic flaws. The kinetic results were analyzed using a computer technique which permits a very detailed examination of various kinetic models. This reveals that the “induction period” (α < ~ 0.01) is very complex and comprises a desorption step, a linear process, an exponential process, and the beginnings of an Avrami process. The latter three processes are identified with (i) the inward growth of rapidly formed surface nuclei, (ii) “branching” of surface nuclei, and (iii) nucleation in the bulk crystal. Kinetic parameters are obtained for these three processes and also for the growth of nuclei in the bulk crystal. This model fits the kinetic data over the complete range of α(0–1), or 1 × 10?5 < α < 1 if the desorption step is not included. The mechanism of the reaction and possible effects on this of Ba2+ and SO2?4 doping are discussed briefly.  相似文献   

12.
13.
The thermal decomposition of ammonium fluoromanganates (III) has been investigated in air and argon by simultaneous thermogravimetry and differential thermal analysis. Chemical analysis, X-ray powder data, and infrared spectra have been employed to characterise the intermediate and final products. The thermal decomposition can be described by the sequence (NH43MnF6 → (NH4)2MnF5 → NH4MnF4 → MnF2. Although penta- and tetra-fluoromanganates are well-defined compounds, the intermediate states could not be separated. In addition, a high temperature form of ammonium hexafluoromanganate has been observed.  相似文献   

14.
Results of a thermal analysis of a system constituted by ammonium nitrate and a three-component additive with Mg(NO3)2 as a promising ecologically clean oxidizing agent for high-energy condensed systems are presented.  相似文献   

15.
《Chemical physics letters》1985,113(4):399-402
The thermal decomposition of formyl fluoride in Ar has been studied behind shock waves over the temperature range 1160–1480 K and the total density range (7.18–18.6) × 10−6 mol cm−3. The decomposition was monitored by means of IR emission from the CH stretching of the reactant and the fundamental band of the CO produced. The decomposition was found to be molecular elimination producing HF and CO and the process proceeded in the low-pressure region under the present conditions. The second-order rate constant was expressed as k/Ar = 1014,74 exp(−35.2 kcal mol−1/RT) cm3 mol−1 s−1. Applying the RRKM strong collision theory, the value of the threshold energy and the collision efficiency were discussed.  相似文献   

16.
17.
The thermal decomposition of some mixed uranyl complexes with Schiff bases and DMSO, EtOH or (Ph)3PO as neutral ligand, were investigated and the corresponding activation energy, E*a, and enthalpy of dissociation, ΔHd, values were calculated.

The results obtained indicate that for the same neutral ligand, the thermal stability of the uranyl complexes is influenced by the Schiff base used; for the same Schiff base, the presence of (Ph)3PO results in a greater thermal stability of the mixed complexes than when the other two neutral ligands are present.  相似文献   


18.
Thermal decomposition of ammonium perchlorate based mixture with fullerenes   总被引:1,自引:0,他引:1  
The effects of fullerenes, including fellerene soot (FS), extracted fullerene soot (EFS) and pure C60 on the thermal decomposition of ammonium perchlorate (AP) compared with traditional carbon black (CB) catalyst has been studied by employing thermogravimetry (TG), differential thermal analysis (DTA), infrared spectroscopy (IR) and ignition temperature experiments. The results showed that the addition of CB and FS to AP reduced the activation energy as well as the temperature at maximum decomposition rate, but that of EFS and pure C60 had little effect on the thermal decomposition of AP, and among all catalysts, FS was the best one.  相似文献   

19.
20.
The thermal decomposition properties and the heat of combustion (ΔH) of samples with different ammonium perchlorate (AP)/double base propellant (DB) mass ratios under argon atmosphere were studied by the thermogravimetry–differential scanning calorimetry–mass spectrometry–Fourier transform infrared spectroscopy (TG–DSC–MS–FTIR) and automatic calorimeter method. The results show that decomposition process of AP/DB samples in negative and zero oxygen balance (OB) is different from that in positive OB. With the increasing of AP in the AP/DB samples, the decomposition of the samples becomes more and more severe. When the OB of the samples is positive, the phenomenon of deflagration or explosion could be observed in the decomposition process. The sample with OB = 0 has the greatest heat of combustion.  相似文献   

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