Aluminum - Fluoropolymer Combustion

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1 Aluminum - Fluoropolymer Combustion Prof. Michelle Pantoya J. W. Wright Regents Endowed Chair Professor Mechanical Engineering Department Acknowledgements: Army Research Office Dr. Ralph Anthenien Office of Naval Research Dr. Cliff Bedford October 2014

2 Overview Vision - Promote cleaner, safer, and more effective energetic composites through an understanding of basic combustion behaviors. Objective - Examine surface chemistry promoting Al reactivity with fluoropolymers Reaction Kinetics Synthesis Strategies 2

3 Al Powder Production < 25 microns Amorphous Shell Crystalline Core High purity Al introduced to a heated ceramic (2000 C) with an inert (Ar) gas flow. Vapor phase Al travels, nucleates, and coagulates Cools and crystalizes as a solid Oxygen introduced after solidification (<660 C). Typically in amorphous phase (~440 C - ambient) 3 Pesiri et al J. Pyro 2004 Johnson & Higa MRS Proccedings 1996 Kerns et al. Mat Sci. & Eng 2004 Amorphous g d/q a g-phase starts at 440 C

4 Exothermic Surface Chemistry Al-F Kinetics of Al + F Reactions Equilibrium Reactions DSC-TGA Analysis PTFE 50nm Al 10 mg samples 4 Osborne et al. Comb Sci Tech 2007 Dean et al. Thermochimica Acta 2009 Mulamba et al. Applied Surface Sci. 2014

5 50nm Al / PTFE (70/30) Fluorination of Al core Decomposition of PTFE PIR: Fluorination of Al 2 O 3 shell PTFE melt: 322 C Al melt 5 Osborne et al. Comb Sci Tech 2007

6 15-30% PTFE: 50 nm Al 30% PTFE PIR same for all stoichiometries 25% PTFE 20% PTFE 15% PTFE 6

7 Nano vs Micron Al - PTFE Kinetics Mass change Heat flow 50nm Al / Teflon 70/30 Nano-Al/Teflon more energetic than micron- Al/Teflon Nano-Al/Teflon shows 2- stage reaction Nano-Al/Teflon lost only 6% of mass Micron-Al/Teflon lost 25% of its mass Micron-Al/Teflon left largely unreacted Osborne et al. Comb Sci Tech um Al / Teflon 70/30 7

8 Hydroxyl Bonds to Alumina Surface III FT-IR of g-al 2 O 3 - Hydroxyl groups bound to surface in many ways II o Tetrahedrially coordinated aluminum (I) I g-al 2 O 3 o Two alumina ions with one in the tetrahedral coordination and the other in octahedral coordination (II) o Three octahedrally coordinated aluminum ions (III) F-Treated g-al 2 O 3 Sarbak Cryst. Res. Tech Peri J. Phys. Chem

9 Role of surface hydroxyl groups To test the PIR dependence on OH surface groups, Al 2 O 3 was calcined at 550 C to decrease OH surface sites and then mixed with Teflon and analyzed. Smaller exotherm signifies less Al 2 O 3 fluorination, supporting reliance of Al 2 O 3 fluorination on surface OH groups. o Hydrated Al 2 O 3 used in water treatment fluoride extraction Extent of substitution depends on hydration of alumina Saniger et al., J. of Fluorine Chem., 88 (1998) Al 2 O 3 /Teflon Calcined Al 2 O 3 /Teflon Fluorine OH substitution Sarbak, Cryst. Res. Technol., 32 (4) (1997)

10 Exothermic Surface Reactions: Pre-Ignition Reaction (PIR) AlF 3 reaction is exothermic starting at 400 C (b-alf 3 ) AlF 3 transition from b to a phase causes exothermic peak at 552 C. o Also corresponds to Aloxidation contributing to overall heat of combustion 15nm g-al 2 O 3 +Teflon b-alf 3 formed b a 10

11 11 PIR effects on Teflon degradation PIR causes Teflon to degrade at lower temperatures In case of g-al 2 O 3 - Teflon o 60 C lower onset temperature. Stripping fluoride ions from polymer during PIR causes chain to become unstable, requiring less energy to degrade. Al 2 O 3 /Teflon Mass change Teflon 60 C

12 Al/Teflon Thermal Degradation ~ 400 C C ~ 550 C 1. Fluorination of amorphous Al 2 O 3 via surface OH groups 2. Teflon becomes unstable and degrades 3. Al 2 O 3 g crystallization enables diffusion of fluoride ions to Al core for fluorination 12

13 Loose powder confined in a tube: Energy Propagation Acrylic tubing 10.0 cm length Instrumented with detectors spaced 1 cm apart 6 photo-detectors 6 piezo-crystal pressure sensors The Bockmon Tube Bockmon et al, J of Applied Physics 2005

14 Flame Speeds Flame speed - optic signals & high speed camera Pressure history mode of propagation & t rxn Bockmon et al, Journal of Applied Physics 2005

15 Affect of Fluoropolymer Chemistry Al/MP 1600 Al/MP 1000 Al/MP 1400 Al/MP 1400 Al/MP 1000 Al/MP 1600 Al/MP DuPont Zonyl MP PTFE vary in chain length MP1100 < MP1600 < MP1000< MP1400 Also in melt temperature 324 < 328 < 330 < 332 C Particle size constant ~10m PIR only observed for longer chain lengths Flame speed higher for PIR kinetics Mulamba et al. Ap. Surf. Sci

16 Flame speed (m/s) PIR and Flame Speed: Al + MoO 3 + PTFE 9 Al+MoO Al + MoO 3 + 5%PTFE %PTFE Al + MoO % PTFE

17 Flame Propagation Velocity (m/s) Aluminum + DuPont Zonyl MP Hexane 17 Hexane 165 m/s Nonpolar Isopropanol Isopropanol 406 m/s Protic Acetone Acetone 460 m/s Aprotic

18 -OH bonding via FTIR Wavenumbers for OH IR absorption are well defined Type Wavenumber Range Net charge on -OH Basicity is as follows: A > D > B > E > C No. of oxide nearest neighbor A B C D E Knozinger and Ratnasamy Catal. Rev. Sci. Eng Peri J. Phys. Chem. 1965

19 Analysis: FTIR A b s o r b s n c e U n i t s Hexane Type D OH bonds Isopropa nol Acetone Wavenumber (1/cm) A b s o r b s n c e U n i t s Type C OH bonds Hexane Isoprop anol Acetone Acetone and Isopropanol are strong Lewis acids & promote OH growth on the alumina surface Type D OH bond Strong Lewis Base Wavenumber (1/cm)

20 Analysis: Review Effect of Solvent Energy propagation rates are significantly affected by the solvent used to mix Al + PTFE Flame speeds Acetone > Isoporponal > Hexane No difference in physical mixing (SEM) Acetone and Isopropanol are strong Lewis acids & promote OH growth on the alumina surface Type D OH bond Strong Lewis Base From Sarbak s study: OH bonds on the surface of Al2O3 are dislodged by F produces exothermic chemistry Observed to be a rate determining step in energy propagation Greater contribution of OH from Acetone and Isopropanol may promote Al + PTFE reactivity By introducing more surface sites that catalyze the PTFE + Al reaction 20

21 Flexible Free-Standing Al-M x O y -F blends Develop deposition method for thin film thermites. Started with Mg-MnO based thermites Al-MoO 3 also successful Binder-Solvent systems: PVDF-NMP Viton-Acetone Paraffin Paraffin-Xylene Viton PVDF H H H H F H F F F H F H C C C C C C C C C C C C n H H H H n F H F CF3 n F H F H Films are cast using a double blade film applicator 21 Meeks et al. Combustion and Flame 2014

22 SEM Images Cross Section (1% PVDF, 40% Solids, ER:1, 4.39 mm) 22 Meeks et al. Combustion and Flame 2014

23 Characterizations 23 Meeks et al. Combustion and Flame 2014

24 Flame Speeds: Mg-MnO 2 -PVDF Mg-MnO 2 -PVDF most effective for preparation as a thin film coating Greater homogeneity of the mixture Increasing PVDF concentration resulted in higher heat of combustion Decreased flame speeds 24 Meeks et al. Combustion and Flame 2014

25 Al-I 2 O 5 PIR I 2 O 5 Kinetics I2O5 Heat Flow Reaction Stage Dissociation Δ r H Onset Temperature Stage A Endotherm I 2 O 5 IO 2 + IO o C Stage B Exotherm I 2 O 3 + O o C Stage C Endotherm IO 2 + IO o C Stage D Exotherm I 2 + O o C 25 Mulamba et al. J. Nanoparticle Research 2014 Chaudhuri et al. J. Chem Phys 2013.

26 Al/I2O5 Heat Flow and Mass loss PIR PIR occurs at lower temp for I 2 O 5 than C 2 F 2 26 Mulamba et al J. Nano Research 2014

27 Al2O3/I2O5 :Exothermic Surface Chemistry 27 Mulamba et al J. Nano. Research 2014

28 Leaner mixtures delay onset of PIR 28 Mulamba et al J. Nano Research 2014

29 Varying Heating Rates Consistent Stoichiometry A 10 o C min -1 B 20 o C min -1 C 25 o C min -1 D 30 o C min -1 E 40 o C min Consistent PIR activation post 25 o C min -1 Activation energy (PIR) = 1.42 kj/g Mulamba et al J. Nano. Research 2014

30 Conclusions Fundamental Al-F surface chemistry analyzed o PIR caused by fluorination of the oxide shell via surface OH Fluoropolymer stability / Al surface area / hydroxyl concentration Newly synthesized Al-F based formulations show potential for a variety of tailorable composites o Fibers o Moldable flexible materials o Films Al-I exhibits similar surface exotherms - PIR o Heating rate governs manifestation o Stoichiometry governs onset o Activation energy related to propagation speed 30

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