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Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase

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Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase NATO UNCLASSIFIED Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase Dr. Manfred Bohn Fraunhofer-Institut für Chemische Technologie (ICT) Postfach 1240 D-76318 Pfinztal-Berghausen GERMANY e-mail: [email protected] ABSTRACT Ammonium dinitramide (ADN) is one of the substances, which are seen to be able to replace ammonium perchlorate (AP) as oxidizer in rocket propellants. Some of the performance data in comparison to AP substantiate this suggestion (values for AP in brackets). It has a good oxygen balance of +25.8% (+34%), a more positive enthalpy of formation, -1208 J/g (-2518 J/g) and a higher heat of explosion as AP, 3337 J/g (1972 J/g). An additional advantage is that the reaction products of ADN are free of signature. One drawback of ADN clearly is the much lower thermal stability than that of AP, together with the relatively low melting point between 92 and 94°C. But the lower stability must not exclude its application in some types of rocket systems. The intrinsic stability of ADN is not much lower than that of unstabilized nitrocellulose. If it would be possible to find stabilizers, ADN can be considered as a substitute candidate for AP. An extensive investigation was made with eight substances to find out their stabilization effect on ADN. The ADN samples were mixed intensively with an amount of 2 mol-% each of these chemicals. The experimental methods used to determine the stabilization effect have been mass loss as function of time and temperature, 65°C, 70°C, 75°C, 80°C, and adiabatic self heating. ADN without additives decomposes autocatalytically. All tested chemicals can prevent the autocatalytic increase in decomposition activity, some of them do it well. The stabilization ability changes somewhat with temperature. With well stabilized solid phase ADN the decomposition of the rate determining step is the N-N bond cleavage in the dinitramide anion. In unstabilized ADN the protonation of hydrogen dinitramide accelerates its decomposition autocatalytically. 1.0 INTRODUCTION Ammonium dinitramide (ADN) is the ammonium salt of the dinitramine HN(NO2)2, HDN, which can be named hydrogen dinitramine when seen as covalent compound or hydrogen dinitramide when seen as ionic compound. HDN is a very strong acid in water. In pure form it decomposes immediately explosive − like. The anion N(NO2)2 has experienced some other names: dinitraminate and dinitramidate. There is some plausibility for using these names but the same holds for naming it dinitramide. So here with the latter nomenclature will be continued. ADN has a potential as performing oxidizer and may replace ammonium perchlorate (AP). The chemical structure formula of ADN can be seen in Fig. 1. In the solid phase it is present in the ionic form. The basic performance data are listed in Table 1, together with those of AP, ammonium nitrate (AN) and hydrazinium nitroformate (HNF). ADN has a high positive oxygen 0 balance of + 25.8%, the enthalpy of formation ∆Hf is more positive than the one of AP and the intrinsic heat of explosion of ADN is higher than the one of AP. ADN is chlorine free and a reduction of signature in the exhaust of rocket motors is achievable easier than with AP. Specific impulses ISP of > 250 Ns/N seem reachable. But ADN is intrinsically instable in the range of the usual service temperatures. Its melting temperature is with about 92°C relatively low and lower melting mixtures and eutectics with Paper presented at the RTO AVT Specialists’ Meeting on “Advances in Rocket Performance Life and Disposal”, held in Aalborg, Denmark, 23-26 September 2002, and published in RTO-MP-091. RTO-MP-091 9 - 1 NATO UNCLASSIFIED NATO UNCLASSIFIED Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase ammonium nitrate below 80°C have to be regarded. Chemically ADN is an aggressive and strong nitration and oxidation agent. The compatibility between ADN and other components in a formulation is therefore demanding. Therewith two questions are essential: • Can ADN be stabilized reliably ? • Are the compatibility demands reachable ? This paper deals only with the first question. NO2 + NH4 N NO2 Figure 1: Chemical Structure Formula of ADN (Ammonium Dinitramide). In the solid phase ADN is present in ionic form as ammonium cation and dinitramide anion. Table 1: Performance data of the oxidizers ADN, AP, AN and HNF. The values of the heats of explosion and gas volumes have been calculated by the ICT-Thermo-dynamic-Code. The other data are from the ICT-Thermochemical Data Base [1]. substance molar O2-balance enthalpy of formation QEX QEX, density gas TM 0 mass ∆Hf wg *) wl *} vol. *] g/mol % kJ/mol J/g J/g J/g g/cm3 cm3/g °C ADN 124.056 + 25.8 − 149.8 − 1207.5 2668 3337 1.81 592 92.9 AP 117.489 + 34.0 − 295.8 − 2517.7 1396 1972 1.95 533 130; D AN 80.043 + 20.0 − 365.6 − 4567.5 1441 2479 1.73 459 169.9 HNF 183.081 + 13.1 − 76.9 − 420.0 5012 5579 1.91 568 124; D *) wg: QEX value with water as gas. *} wl: QEX value with water as liquid at 20°C. *] gas volume of the substance with thermodynamically controlled combustion, at 25°C without water. D in the column of TM means decomposition at the given temperature, which may vary with the sensitivity of the observation. In [2] a further value of −148 ± 10 kJ/mol for the heat of formation at constant volume is reported for 0 ADN. With this the value of −162.8 kJ/mol (−1312.3 J/g) results for the enthalpy of formation ∆Hf at standard conditions. Hydrogen was used instead of oxygen to burn ADN in the bomb calorimeter. 2.0 METHODS AND MATERIALS USED The following measurement methods have been used to determine the stabilizing effect of an added substance in comparison to the ADN alone. 9 - 2 RTO-MP-091 NATO UNCLASSIFIED NATO UNCLASSIFIED Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase • Mass loss measurements ADN without and with additives, three samples in parallel, each 1 to 2 grams at temperatures of 65°C, 70°C, 75°C, 80°C. The samples were aged in pyrex glass vials inserted in aluminium block ovens. The temperature constancy was very good by PID control. Also in long terms the constancy was at least ± 0.3°C. Therefore the temperature was additionally controlled by calibrated devices and sensors independent from those of the PID controller. The mass loss is proportional to the ‘global’ conversion of the sample. • Adiabatic self heating The adiabatic self heat rate was determined with an ARCTM (Accelerating Rate Calorimeter). Details about this method can be found in [3]. The adiabatic self heat rate is proportional to the ‘global’ reaction rate of the sample. The measurement temperatures are in the range of 90°C to 200°C. With these methods two different probings of the samples have been achieved: Method Probing Mass loss sum of split-off decomp. gases (absolute effect) Adiabatic self heating sum of heats of reaction (net effect) The use of methods with different probing assures the results [4]. The ADN used was manufactured at ICT in 1998. Eight substances S have been applied as additives to test their stabilization effect on ADN. The amounts in the mixtures have been number-normalized that means a constant molar percentage of a substance S was added to ADN, here two mol-%. The mixtures have been mixed intensively with a three axis moving mixer for one hour. A further ADN lot made at ICT and a lot from a company are compared with non-stabilized ADN-ICT-1998. 3.0 RESULTS 3.1 Mass Loss 4 ML [%] ADN-ICT-1998 3.5 non-stabilized 3 65°C 70°C 2.5 75°C 2 80°C 1.5 1 0.5 time [d] 0 0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400 Figure 2: Mass Loss of Unstabilized ADN-ICT-1998 at Temperatures between 65°C and 80°C. RTO-MP-091 9 - 3 NATO UNCLASSIFIED NATO UNCLASSIFIED Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase Fig. 2 shows the mass loss of ADN alone at the temperatures 65°C, 70°C, 75°C and 80°C. Especially at 80°C and 75°C the autocatalytic type increase of mass loss can be seen well in the scaling of the figure. At 80°C the steady increase of the mass loss starts at about 10 to 12 days. Sometimes the ADN liquefies after such times already and the mass loss increases very strong in a catastrophic like manner, Fig. 3. Additional acceleration of the decomposition is induced by liquefaction. It is therefore necessary to stabilize ADN. 0.8 ML [%] Comparison of some ADN lots 0.7 ML measurements at 80°C 0.6 ICT 3/1998 ICT 9/2000 0.5 Company 1998 0.4 0.3 0.2 0.1 time [d] 0 0 2 4 6 8 1012141618202224 Figure 3: Comparison of Three ADN Lots. ICT 9/2000 behaves qualitatively similar to ADN of a company, measured in 1998. For the application of ADN in formulations the primary product after production is rarely suitable. The ADN should be prilled, means transformed to sphere-like shape. By this process, done at ICT, the stability of ADN is only lowered somewhat, see Fig. 4. 8 ML [%] ADN-ICT-1998 7 non-stabilized comparison unprilled - prilled 6 80°C 5 75°C 70°C 4 80°C-Prill 75°C-Prill 3 70°C-Prill 2 1 time [d] 0 0 25 50 75 100 125 150 175 200 225 250 275 300 325 -1 Figure 4: Comparison of Unprilled and Prilled ADN-ICT-1998.
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