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Sejin Kwon
Korea Advanced Institute of Science and Technology
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measurements in the microreactor and correlated with the ignition delays that were separately measured by drop tests
with high-test peroxide. The reaction rate measurements were fully compatible with the drop test results and proved
to be useful as an alternative method for the selection of hypergolic propellants by ignition characteristics.
D. MEMS Reactor Test Setup need to take additional safety precautions. In this work, the oxidizer
As shown in Fig. 3, a dual-channel syringe pump was used to to fuel mass ratio was approximately 1.1–1.4, depending on the
Downloaded by KOREA ADVANCED INST OF SCIENCE on October 19, 2016 | http://arc.aiaa.org | DOI: 10.2514/1.A33634
simultaneously supply the reactants into the microreactor at a specific density of the fuels; this was a fuel-rich environment. The reactants
volume flow rate. Because the dual-channel syringe pump was flowed in the channels fabricated in the MEMS reactor at a
introduced, the shear rate between the two streams should be the same microfluidic scale and contacted at a designated point. The reactants
regardless of the flow rate. It is therefore expected that the rate of continued to react until they reached the outlet, and therefore the
diffusive transport can play a major role to mix the two streams in a temperature rise measured at the outlet can be regarded as the final
liquid-phase reaction, independent of shear-driven convective reaction temperature in this microreactor system. An open-end k-type
transport. The fuel and oxidizer were supplied from 5 to 50 ml∕h, thermocouple was located at the outlet to gauge the temperature rise.
which was the usable range of this microreactor test system. In the
microreactor tests, the Reynolds number of the flows ranged from 7 to
130, depending on the volume flow rate of the propellants. To prevent III. Results and Discussion
evaporation and boiling by the reaction heat, a low-concentration A. Ignition Delay of Nontoxic Hypergolic Propellants in Drop Tests
hydrogen peroxide at 34.5 wt % was used as a reference oxidizer. The An oxidizer droplet softly fell down to the fuel pool in all cases,
low-concentration hydrogen peroxide was produced by diluting HTP which indicates that hypergolic ignition occurred in a fuel-rich
with distilled water. Another benefit of using low-concentration environment. The diameter of the droplet was approximately 3.2 mm,
hydrogen peroxide was to avoid the occurrence of hypergolic ignition and the drop height was almost 12 cm from the surface of the pool.
in the flow channels of the microreactor, and there was therefore no Figures 4 and 5 present a series of consecutive high-speed images that
Fig. 3 Schematic diagram of the apparatus for the MEMS reactor tests.
Fig. 4 High-speed images of hypergolic ignition of reactive fuel 1 with a 90 wt % H2 O2 oxidizer droplet.
4 Article in Advance / KANG, HUH, AND KWON
Fig. 5 High-speed images of hypergolic ignition of catalytic fuel 2 with a 95 wt % H2 O2 oxidizer droplet.
contact of an oxidizer droplet on the surface of the pool, and the flame
spread outward to cover the entire liquid surface. Hypergolic ignition
was manifestly achieved for the two different prepared fuels with the
HTP. It had been already verified that catalytic fuel 1 (block 0) has
hypergolic properties with HTP [12].
The drop tests suggest that distinguishable ignition mechanisms
occurred between the catalytic fuels and the reactive fuel. When a
catalytic fuel came into contact with the oxidizer, the catalyst
dispersed in the catalytic fuel began to decompose the oxidizer,
thereby vigorously generating a reactive vapor above the surface of
the fuel. In the case of reactive fuel 1, a strong reducing agent
dissolved in the fuel directly reacted to the oxidizer and triggered
ignition via a reduction-oxidation reaction that was highly energetic
and immediate.
With a high concentration of hydrogen peroxide, the chemical
reactions became intense. Table 3 represents the reduction in the
ignition delays of the fuels as the concentration of hydrogen peroxide
was increased. Reactive fuel 1 had the shortest period of ignition Fig. 6 Variations in outlet temperature of nontoxic hypergolic fuels with
34.5 wt % H2 O2 at 15 ml∕h.
delay, which was attributed to the reduction-oxidation reaction that
provided shorter reaction paths than those of catalytic ignition [20].
Catalytic fuel 1 (block 0) ignited faster than catalytic fuel 2 because,
like H2 O2 , catalytic fuel 1 is a polar solvent (methanol). On the other incompletely reacted catalytic reactants continued to flow down from
hand, catalytic fuel 2 had the longest delay time because it is upstream. On the other hand, the fluctuations in the temperature
kerosene-based fuel and has relatively low polarity, which made it profile of reactive fuel 1 might have been caused by minute bubbles
more difficult to penetrate the oxidizer into the fuel. that were generated in the flow channels by exothermic reactions,
where the reaction temperature reached approximately 100°C. The
B. Quantitative Interpretation of the MEMS Reactor Test Results extent of the fluctuations could have been related to the intensity of
The main purpose of the MEMS reactor tests was to estimate the the chemical reactions that participated in the hypergolic interactions.
activation parameters involved in the liquid-phase hypergolic Figure 7 shows the reaction temperatures at the outlet in the steady
reactions and verify the correlation between the parameters and the state, which depended on the change in the volume flow rate of the
actual ignition performance of the hypergolic propellants. The results reactants. The reaction temperature rose as the volume flow rate was
from the microreactor tests are presented in Fig. 6. Each fuel increased. This is because the pressure inside of the flow channel was
exhibited a different rate of reaction and temperature rise at the outlet, locally raised as a result of the increase in the flow rates at the specific
even under the same conditions. After the transient response was volume. The local pressure rise could have encouraged one fluid to
examined, the profile of the reaction temperature reached a specific penetrate into the other, so that the contact surface between the two
value without wide variation, representing a steady-state condition. fluids became larger on a molecular scale. Thus, the fluids had more
For the catalytic fuels, once the reaction temperature rose to the peak opportunity to interact with each other, which led to more exothermic
value, it decreased slowly and became stable. In the case of reactive reactions. The final reaction temperatures of reactive fuel 1 were
fuel 1, the transient state was remarkably shorter than those of the higher than those of the catalytic fuels. To sustain stable combustion,
catalytic fuels. After the transient state, the reaction temperature was the fuel had to generate more energy than the global heat loss. It
maintained above the first peak value, and marginal fluctuations were therefore was expected that the catalytic fuels required more mass to
observed. There are two reasons why the reaction temperatures of produce enough energy to overcome the large amount of heat lost to
the catalytic fuels decreased after the transient state; considerable the atmosphere from the microreactor. Given that reactive fuel 1
heat losses between the reactor and atmosphere occurred, and produced the largest amount of heat energy under the same
Unit, ms 90 wt % 92 wt % 94 wt % 95 wt % 98 wt %
Reactive fuel 1 15.6 (2.4) No data 10.5 (2.2) 6.5 (1.4) 5 (0.8)
Catalytic fuel 1 (block 0) [12] No data 218 (99.8) 22.5 (2.5) No data 13.2 (1.5)
Catalytic fuel 2 No ignition No ignition 130 (13.5) 92 (8.5) 74.5 (5.5)
a
The standard deviations are given in parentheses.
Article in Advance / KANG, HUH, AND KWON 5
Downloaded by KOREA ADVANCED INST OF SCIENCE on October 19, 2016 | http://arc.aiaa.org | DOI: 10.2514/1.A33634
Ea 1 §
ln k ln A − (2) Data available online at http://employees.csbsju.edu/cschaller/Reactivity/
R T MLnSub/lsTSparam.htm [retrieved 13 September 2016].
6 Article in Advance / KANG, HUH, AND KWON
Table 4 Experimental data of the Arrhenius plots and Prospects,” Progress in Aerospace Sciences, Vol. 71, Nov. 2014,
pp. 128–149.
Activation energy Entropy of activation doi:10.1016/j.paerosci.2014.08.001
Ea ,a kJ∕mol ΔS,a J∕K ⋅ mol [7] Alfano, A. J., Mills, J. D., and Vaghjiani, G. L., “Highly Accurate
Reactive fuel 1 35.4 60.5 Ignition Delay Apparatus for Hypergolic Fuel Research,” Review of
Catalytic fuel 1 (block 0) 72.9 171.7 Scientific Instruments, Vol. 77, No. 4, 2006, Paper 045109.
Catalytic fuel 2 83.6 198.3 doi:10.1063/1.2188909
[8] Dambach, E. M., Cho, K. Y., Pourpoint, T. L., and Heister, S. D.,
a
Ea and ΔS ln A × R were obtained from the plots of the logarithm of the “Ignition of Advanced Hypergolic Propellants,” Proceedings of 46th
Arrhenius equations [24]. AIAA/ASME/SAE/ASEE Joint Propulsion Conference and Exhibit, AIAA
Paper 2010-6984, Nashville, TN, July 2010.
[9] Farmer, M. J., Mays, L. O., Hampton, C. S., and Smith, J. E., “Reaction
Rates for Hypergolic Propellants Using Chemical Delay Times,”
IV. Conclusions Journal of Propulsion and Power, Vol. 20, No. 2, 2004, pp. 372–376.
An experimental approach to evaluate the rates of hypergolic doi:10.2514/1.9262
ignition liquid-phase chemical reactions should be considered for [10] Saksena, P., Tadigadapa, S., and Yetter, R. A., “Study of Hypergolic
nontoxic liquid hypergolic propellants. The reaction rate is an important Propellants Using Micro-Reactors,” Proceedings of 15th International
factor that predominantly influences the initiation of the hypergolic Conference on Miniaturized Systems for Chemistry and Life Sciences,
Seattle, Washington, D.C., Oct. 2011.
Downloaded by KOREA ADVANCED INST OF SCIENCE on October 19, 2016 | http://arc.aiaa.org | DOI: 10.2514/1.A33634