Sanjana Datta - Reaction Dynamics and Probability Study of Fluoroelastomer Coated Aluminum Particles Seeded in A Viton-Acetone Droplet

Reaction dynamics and probability study of fluoroelastomer coated aluminum particles seeded in a Viton-Acetone droplet
by
Sanjana Datta, B.S.M.E. A Thesis In MECHANICAL ENGINEERING Submitted to the Graduate Faculty of Texas Tech University in Partial Fulfillment of the Requirements for the Degree of MASTER OF SCIENCES IN MECHANICAL ENGINEERING Approved Dr. Michelle Pantoya Chairperson of the Committee Dr. Stephen Ekwaro-Osire Dr. Sukalyan Bhattacharya
Fred Hartmeister Dean of the Graduate School
May, 2010
Copyright 2010, Sanjana Datta
Texas Tech University, Sanjana Datta, May 2010
ACKNOWLEDGMENTS I am thankful to everyone who has helped me accomplish so much during my time at Texas Tech University. Specifically, I am thankful to Dr. Michelle Pantoya for her continuous support and guidance during the past two years. Thank you Dr. Ekwaro-Osire and Dr. Bhattacharya for your helpful discussions. I would like to acknowledge Texas Tech Imaging Center for allowing me to operate their SEM instrument. Additionally, I would like to thank past and present members of the combustion lab for their help, especially Shawn Stacy for his help with real code. I would like to thank Dr. Jharna Chaudhuri and the Mechanical Engineering department for providing financial assistance when there was a need. In addition, I am extremely grateful to the AT&T Foundation for awarding me the AT&T Chancellors Fellowship, which helped fund my education during my time at Texas Tech. I am exceptionally thankful to my parents, Amlan and Soma, and my fianc, Josh for all the support and encouragement to pursue my goals and never give up. They have been by my side through thick and thin.
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TABLE OF CONTENTS ACKNOWLEDGEMENTS ................................................................................ ii ABSTRACT ..................................................................................................... v LIST OF TABLES .......................................................................................... vii LIST OF FIGURES........................................................................................ viii NOMENCLATURE .......................................................................................... xi 1. INTRODUCTION ........................................................................................ 1 1.1. MELT DISPERSION THEORY ............................................................. 1 1.2. NANO-ENERGETIC MATERIAL (nEM) ............................................... 2 1.3. COATING WITH A BINDER ................................................................. 4 1.4. STATISTICAL STUDY.......................................................................... 5 1.5. OBJECTIVE ......................................................................................... 6 2. METHODOLOGY ....................................................................................... 8 2.1. SAMPLE PREPARATION .................................................................... 8 2.2. SETUP OVERVIEW ........................................................................... 13 2.3. DROPLET APPARATUS .................................................................... 14 2.4. TESTING PROCEDURE .................................................................... 18 3. RESULTS ................................................................................................. 20 3.1. EXPERIMENTAL RESULTS .............................................................. 20 3.2. UNCERTAINITY ANALYSIS .............................................................. 26 4. DISCUSSION............................................................................................ 28
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4.1. SIMPLE HEAT TRANSFER MODEL .................................................. 30 4.11. ASSUMPTIONS ........................................................................ 30 4.12. PHYSICAL AND CHEMICAL PROPERTIES ............................ 30 4.13. GOVERNING EQUATIONS ...................................................... 32 4.14. DISCUSSION OF THE DN MODEL.......................................... 32 4.2. PROBABILISTIC ANALYSIS .............................................................. 34 4.21. DETERMINATION OF PROBABILITY DISTRIBUTION............ 35 4.22. LIMIT-STATE FUNCTION ........................................................ 37 4.23. NESSUS ANALYSIS AND RESULTS....................................... 38 4.24. DISCUSSION OF NESSUS RESULTS .................................... 41 5. CONCLUSIONS ....................................................................................... 43 6. SUGGESTED FUTURE WORK................................................................ 44 REFERENCES ............................................................................................... 45 APPENDICES ................................................................................................ 48 A. ADDITIONAL GRAPHS OF ELLIPSOIDAL DIAMETER AS A FUNCTION OF TIME FROM A VITON A ACETONE EXPERIMENT ..... 48 B. NORMALIZED DROPLET DIAMETER GRAPHS FOR VITON AND ACETONE ............................................................................................... 51 C. ADDITIONAL NESSUS ANALYSIS DATA .............................................. 52 D. OUTPUT DATA FOR DIFFERENT TESTS .............................................. 54 E. VALUES OF Dn FOR THE KOLMOGOROV-SMIRNOV TEST ............... 60
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ABSTRACT The fluoroelastomer, Viton A (C5H3.5F6.5), is a common binder for energetic material composites which can be dissolved in acetone and mixed with solid metal fuel particles, such as aluminum. The slurry can be molded into any configuration and the acetone is evaporated off leaving a solid homogeneous reactant mixture. Fundamentally understanding the reaction dynamics of acetone, Viton A, and aluminum is useful for not only consolidating reactants but also for the potential to use nano-sized aluminum in liquid combustion applications. The objective of this study is to examine acetone-Viton A droplet burning as a function of aluminum fuel particle size and concentration. A diagnostic was developed that suspends the multiphase 3mm droplet on a fiber and enables droplet surface regression rates to be monitored with a high speed video camera. Results show that acetone combined with Viton A (5%) and either 2.5% micron aluminum (10-14 m) or nano alumimum (80 nm) burned with two distinct stages. But, acetone combined with Viton A and more than 5% nano aluminum burned with a distinct 3-stage behavior. The three stages are described as evaporation, burning/combustion, and burning of residue with a distinct flame. A probabilistic analysis was performed using NESSUS software to determine the occurrence of the third stage in the multicomponent droplets. Addition of micron aluminum to the Viton A and acetone droplet decreases the burn rate 82% when compared to Viton A and acetone droplets with nano aluminum
particles The probability of the third stage occurring in Viton A and nano aluminum is 1.45% and for Viton A only droplets is 92.1%.
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LIST OF TABLES 2.1 2.2 2.3 Material specifications................................................................. 9 Mass and equivalence ratio for different compositions ............. 11 The five different multicomponent mixtures and their compositions ............................................................................. 12 Compositions of water and acetone samples by volume .......... 16 Comparison of theoretical and experimental evaporation rates of two different samples of water and acetone .......................... 17 The average burn rates and burn times for the droplets ........... 25 Determination of nth power in the Dn Law for acetone-Viton droplets ..................................................................................... 33 The normal and lognormal parameter for 3rd stage Viton/Acetone droplet initial diameter........................................ 36 The K-S Test parameters for 3rd stage Viton/Acetone droplet initial diameter ........................................................................... 36 The normal and lognormal parameter for 2nd stage Viton/Acetone droplet final diameter ......................................... 37 The K-S Test parameters for 2nd stage Viton/Acetone droplet final diameter ............................................................................ 37 The analytical results from NESSUS ........................................ 39
2.4 2.5
3.1 4.1
4.2a
4.2b
4.3a
4.3b
4.4
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LIST OF FIGURES 2.1 2.2 2.3 2.4 2.5 2.6 2.7 SEM micrograph of Viton A ....................................................... 9 Mass scale ................................................................................ 10 a.) Sonicator, b.) Sonicator tip .................................................. 11 SEM micrograph of nm-al particles (uncoated) ......................... 12 SEM micrograph of 2.5% nm-al particles in Viton ..................... 13 Experimental set up ......... 14 front view of the droplet apparatus with suspended droplet of size 2mm...... .................................................14 heated nichrome wire .......... ...18 Still frame images of Viton-acetone droplet reaction dynamics: (a) Stage 1 - evaporation; (b) transition from evaporation to combustion; (c) Stage 2 combustion ..................................... 21 Still frame images of 3rd Stage combustion of carbon residue resulting from Viton-acetone droplet ......................................... 21 iton-acetone and nm-Al droplet regression rate for a) stage 1:evaporation and stage 2: combustion b) stage 3: secondary combustion. .............................................................................. 22 High Speed camera compatible Phantom software with diameter analysis ...................................................................... 24 Comparison of the regression ................................................... 29 Droplets with Nm-Al particles .................................................... 29 The Transfer Number (B) as a function of the Burn Rate Constant (K) from MATLAB ...................................................... 33 CDF of Viton and acetone droplets for 2nd stage final diameter a)without 3rd stage burning b) with 3rd stage burning ................ 38
2.8 3.1
3.2
3.3
3.4
4.1 4.2 4.3
4.4
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4.5
PDF OF Viton and Acetone droplets for 2nd stage final diameter a)without 3rd stage burning b) with 3rd stage burning . 39 The sensitivity graph for Viton and Acetone droplets for probability of occurrence of third stage combustion .................. 40 The sensitivity graph for nm-al, Viton and acetone droplets for probability of occurrence of third stage combustion .................. 41 (Test 1) Ellipsoidal diameter as a function of time..................... 48 (Test 2) Ellipsoidal diameter as a function of time..................... 49 (Test 3) Ellipsoidal diameter as a function of time..................... 49 (Test 4) Ellipsoidal diameter as a function of time..................... 50 (Test 5) Ellipsoidal diameter as a function of time..................... 50 (Test 1) Normalized droplet diameter graphs for Viton and acetone ..................................................................................... 51 (Test 2) Normalized droplet diameter graphs for Viton and acetone ..................................................................................... 51 CDF of nm-al d2 ........................................................................ 52 CDF of nm-al d3 ........................................................................ 53 PDF of nm-al d2 ........................................................................ 53 PDF of nm-al d3 ........................................................................ 53 (Test 1) NESSUS analysis for Viton and acetone droplets ..... 54 (Test 1) NESSUS analysis for Viton, nm-al and acetone droplets ..................................................................................... 55 (Test 2) NESSUS analysis for the Viton and acetone droplet data ........................................................................................... 56 (Test 2) NESSUS analysis for nm-al, Viton and acetone droplet data ............................................................................... 57
4.6
4.7
A.1 A.2 A.3 A.4 A.5 B.1
B.2
C.1 C.2 C.3 C.4 D.1 D.2
D.3
D.4
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D.5
(Test 3) NESSUS analysis for the Viton and acetone droplet data ........................................................................................... 58 (Test 3) NESSUS analysis for all nm-al droplet diameter data .................................................................................................. 59 Values of Dn for the Kolmogorov-Smirnov ............................... 60
D.6
E.1
NOMENCLATURE Bo,q cpg D D2 D3 hc hfg k K m q T Tf Ts V l Transfer, Spalding Number Specific Heat (J/kg-K) Diameter (m) Final 2nd stage diameter for two stage behaviors Final 2nd stage diameter for three stage behaviors Heat of Combustion (J/kg) Latent heat of Vaporization (J/kg) Thermal Conductivity (W/m-K) Burning rate constant (mm2/s) Mass (g) Heat per unit mass (J/kg) Far from the surface temperature (K) Flame Temperature (K) Surface Temperature (K) Volume (cc) Density of the liquid (gm/cc) Oxidizer to fuel stoichiometric ratio (kg/kg) Standard Deviation Mean Lognormal Parameter for mean Lognormal Parameter for standard deviation
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CHAPTER 1 INTRODUCTION 1.1. Melt Dispersion Theory Nanometric particle fuels such as aluminum (Al) demonstrate unique combustion behaviors over their micron scale counterparts. When nanometric Al is combined with a metal oxide or organic or inorganic oxidizer the mixture may be referred to as a nano energetic material (nEM). These nEMs show dramatically increased burn rates and reduced ignition times [1] over micron particle formulations. Several attempts to explain these behaviors have been reported in the literature [1-3]. One theory referred to as the melt dispersion mechanism has been newly introduced as a reaction mechanism based on mechanochemistry principles [2]. The mechanism describes the interaction between a pristine, high-melting temperature alumina shell and the lower-melting temperature aluminum (i.e., Al) core. At high heating rates, the Al core melts and expands exerting pressure on the alumina shell. The shell eventually ruptures by spallating such that unbalanced pressure waves cavitate the molten Al creating a dispersion of liquid Al droplets, which readily oxidize [2]. While no experimental evidence validates this proposed theory on a single particle scale, many macroscopic combustion behaviors have been observed that are consistent with this theory [3].
Macroscopic observations only appear consistent with the melt dispersion mechanism when Al nano-particle shells have not been mechanically altered. For example, compressing the powders into pellets [4] or purposely grinding powders [5] introduces imperfections in the oxide shell which reduce the shell strength under the high pressure load associated with Al core melting. In this way, these imperfections would inactivate the melt dispersion mechanism. A key assumption in the melt dispersion mechanism is that the alumina shell is virtually defect free such that its strength approaches the theoretical maximum [3]. One motivation for this study is to engineer an approach to consolidating powders such that mechanical imperfections to the alumina shell are not introduced. The approach would require the introduction of a liquid to produce a slurry that could be molded into a shaped charge as opposed to pressed. Liquid can be evaporated leaving a consolidate solid particle matrix. In this way, consolidated mixtures could potentially react according to the melt dispersion mechanism such that heightened reactivity may be better exploited.
1.2. Nano-Energetic Material (nEM) There are many applications in which consolidating formulations by pressing and mechanically compacting powders is difficult. For example, a relatively new application for nEMs involves their integration into micro-electromechanical (MEM) devices [6] where nEMs are used as actuators, initiators,
etc. One of the biggest challenges incorporating nEMs into MEM applications is depositing the nEMs into microchannel configurations. Some approaches involve tedious and expensive single molecule placement techniques [7]. These approaches may be difficult and costly to implement on a large scale. However, deposition of a liquid-based slurry of nanoparticle reactants may be a viable approach offering lower cost and large scale-up potential as advantages. For both the exploitation of the melt dispersion mechanism and the MEM applications, the purpose of this study was to experimentally examine the fundamental reaction dynamics of a liquid droplet containing a reactive material formulation that includes nano-Al particles (nm Al). This understanding is effectively a pre-cursor to future efforts devoted to engineering a consolidated reactive material formulation created via a slurry and mold-cast into a shape charge. This fundamental understanding is especially useful in safety protocols where most accidental ignition can occur during the consolidation of the reactive material. In this way, understanding the burning behavior of the multi-phase and multi-component system better predicts the response for auto-ignition and accident scenarios common with nEM consolidation.
1.3. Coating with a Binder To achieve this goal several oxidizers were examined for their solubility in a liquid medium. Viton is a common binder used with Al [8] and was found to dissolve in acetone. Viton (C5H3.5F6.5 ) is a fluoroelastomer in which fluorine acts as an oxidizer. Fluorine is the most electronegative element and readily gains electrons. The Viton-acetone liquid mixture can be combined with Al particles to effectively coat Al particles with Viton after the evaporation of acetone. Hence, in the liquid-solid state, this mixture can be molded into any configuration prior to acetone evaporation. The introduction of this new mold casting consolidation approach using Viton dissolved in acetone presents potential for many applications involving consolidated nEM reaction in which the structural integrity of the particles have not been sacrificed. Coating Al particles with a binder has been reported in several journals. The application of the coating plays a positive role in the propulsion system by reducing the accumulation of slag and erosion of the structural member [9]. Spherical micron sized Al particles combined with an organic binder have been used as a coating for austenitic steel [10]. This aluminized coating acts as a thermal barrier, which protects the blades and vanes of gas turbines from oxidation and corrosion [10] Other uses of binder passivated Al have been reported by Jouet et. al, who showed an enhancement in the rate of Al combustion by the replacing the oxide passivation layer with a fluoropolymer on Al particles [11] . Passivation of Al nanoparticles with molecules containing
oxidizer species such as, perfluorocarboxylic acid, result in energy contributes to the detonation wave produced by explosive formations [11].
1.4. Statistical Study The concept of reliability, probability or risk management has been a thought provoking topic not only among mathematicians, but also among engineers [13]. Since any repeated measurement generates multiple outcomes, no phenomenon can be justified without using the concept of uncertainty, randomness or stochasticity [13]. Though engineers recognize the presence of uncertainty in the analysis and design of engineering systems, traditional approaches consider the use of safety factors which uses uncertain parameters that they consider deterministic [13]. The fact that a safety factor is based on past occurrence does not fully guarantee safety or satisfactory performance, nor does it provide information on the influence of different parameters on safety. Finally, safety factors do not provide information about optimal use of available resources to maximize safety [13]. On the contrary, probabilistic analysis provides this information, required for optimum design [13]. Probabilistic design offers the necessary practicality both for engineering analysis and for the improvement of products, as well as business performance [16]. This can be classified in terms of economics of design, improved reliability, reduced failure cost, increased confidence in analysis, and reduction in the need for prototypes [16]. Probabilistic design differs from the
deterministic approach because it uses the probability of failure instead of using a safety factor. Probabilistic analysis methods are not widely used in the field of combustion, but have been applied in experimental studies on the set of microexplosion for an emulsion droplet [12]. The occurrence of microexplosion is considered random, thus probabilistic analysis was used to predict the stoichasticity of the combustion process [12]. In this model, the Weibull distribution was adopted for successfully predicting the onset probability of microexplosion [12]. A similar model will be employed here to predict the probability of distinctly separate regimes associated with droplet evaporation and combustion.
1.5. Objective The objective of this study is to understand the combustion behavior Al particles material when combined with a Viton A-Acetone solution as a function of the composition and Al particle size. A motivation for this study was secondary to develop a synthesis process which coats Al particles with a fluoroelastomer that may have implications for consolidating high bulk nEM. There has been no previous droplet combustion study on Viton A-Acetone combined with Al. This study is a unique contribution to the field of combustion since it investigates burning behavior of a fluoroelastomer dissolved in an organic compound with nano and micron Al. Additionally, the
study was conducted using an original droplet suspending apparatus that can suspend droplets of approximately 3 mm. The main goals of the current study are to create a diagnostic that can test single or multicomponent droplets, to examine the D2-law applied to droplet evaporation and combustion, of Viton A-acetone solution combined with nano and micron-scale Al particles, and employ a probabilistic analysis that can be used to predict burning behaviors.
CHAPTER 2 METHODOLOGY 2.1. Sample Preparation Multicomponent mixtures were obtained by mixing acetone with 5% mass of Viton A. Viton A was cut into roughly 5 mm pieces and measured to the appropriate mass using the scale shown in Figure 2.1. The small pieces of Viton was placed in acetone and allowed to completely dissolve, which corresponds to roughly 1 day. The acetone was purchased from Mallinckrodt Chemicals and Viton A sheet was purchased from DuPont. The acetone and Viton A were mixed with different Al particle sizes and prepared at various mixture compositions. The nano aluminum particles (80 nm) were purchased from NovaCentrix (Austin, TX) formerly known as Nanotechnologies. These particles are of spherical morphology with 80% active Al content (i.e., 20% is in the form of alumina (Al 2O3), consistent with the passivation shell surrounding the Al core). The micron particles were purchased from Alfa Aesar and have a spherical morphology with 97.5% active Al content (i.e., 2.5% is in the form of alumina (Al 2O3), consistent with the passivation shell surrounding the Al core). The materials are summarized in Table 2.1.
Figure 2.1: SEM micrograph of Viton A
Table 2.1. Material Specifications Material Acetone Aluminum Aluminum Viton Particle Size N/A 80 nm 10-14 m N/A Manufacture Mallinckrodt NovaCentrix Alfa Aesar Dupont Purity 99% 99% 97.5% A(Grade) Form Factor Liquid Spherical Spherical Sheet
Various masses of the different components were measured on a mass scale accurate to 0.1mg (Figure 2.1). The mass of the Viton and Al depends on the desired total mass.
Figure 2.2: Mass Scale
The equivalence ratio () was calculated for different mixtures (shown in Table 2.4). An equivalence ratio () is defines as: (2.1.1) Where mfuel is the mass of the fuel, moxidizer is the oxidizer mass and the subscript st represents the stoichiometric ratio of fuel and mass. The stoichiometric ratio refers to a reaction in which the optimal ratios of fuel and oxidizer are used so that a complete reaction would consume all fuel and oxidizer. The chemically balanced Viton and acetone reaction in pure oxygen is shown in equation 2.1.2.
(2.1.2)
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Table 2.2: Mass and Equivalence ratio for different compositions
1 Acetone Viton Aluminum1

33.3% air
2 10000 500 25 5262.5
3 10000 500 12.5 5256.25
4 10000 500 37.9196429 5268.95982
5 10000 500 0 5250 2.312
10000 500 12.5 5256.25
Aluminum was added to the Viton A and acetone mixture. The samples were placed in the Misonix Sonicator 3000, (Figure 2.2), to break up agglomerates and promote homogeneous mixing of particles. The ultrasonic probe consists of 10 second mixing cycles and 10 second idle time, repeated 3 times for a total process time of 60 seconds.
Figure 2.3 : a) Sonicator b) Sonicator tip
Composition 1,2, and 3 are nm-Al. 4 is micron aluminum composition.
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Table 2.3: The five different multicomponent mixtures and their compositions
Acetone (% mass) 95 95 95 95 95
Viton A (% mass)* 5 5 5 5 5
Nm-Al (% mass)** 0 0 2.5 5.0 7.5
Al (% mass)** 0 2.5 0 0 0
* Viton (%mass) = massviton/massacetone ** Al (%mass) = massAl/massviton
Figure 2.3 and 2.4 are SEM micrographs of nm-Al particles, coated with Viton A and uncoated.
Figure 2.4: SEM micrograph of nm-Al particles (uncoated)
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Figure 2.5: SEM micrograph of 2.5% nm-Al particles in Viton
2.2. Setup Overview The experimental setup is illustrated in figure 2.3. The Phantom IV high speed digital camera was attached is a K2 Long-Distance Microscope (Infinity Photo-Optical Company, Boulder, CO) for higher magnification. A fiber optic light source (Cole Parmer Illuminator, 41720 series) increases the contrast between the droplets and the background. The temperature and relative humidity is monitor was measured with the Digital Hygro Thermometer. The acrylic plate with the nichrome wire was placed underneath the quartz fiber.
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Voltage Source Light Source
Droplet Suspension Apparatus
Droplet Phantom IV w/ K2
Nichrome wire
Figure 2.6: Experimental Set-up
2.3. Droplet Apparatus A quartz fiber droplet suspending apparatus was developed (Figure 2.4). The 1 mm quartz fiber was attached to the suspension apparatus by means of two screws, one at the top and the other at the bottom. The face of the droplet apparatus facing the camera was painted black so that the transparent droplet is easily visible.
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Screw at the bottom
1 mm Quartz Fiber
2 mm water droplet
Figure 2.7: Front view of the droplet apparatus with suspended droplet of size 2 mm
To determine the accuracy and reliability of the current apparatus and diagnostics, a simple water and acetone experiment was set-up to re-create the D2-law model for evaporating droplet [14]. Acetone is an alcohol and evaporates faster than water. The high speed camera used for the experiment has a maximum exposure time of 51s. Acetone expedites the evaporation time of the water droplet hence, it is necessary to use acetone so that the entire evaporation process can be recorded with the high speed camera. Water and acetone droplets of two different compositions were evaluated to find their evaporation rates. The two different compositions were used to create two separate experimental models. This was done to see if both experimental models generated results as predicted by the mathematical D2-law model [14]. If the result from the mathematical model agree with the
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result from the diagnostic model, this original experimental setup can be used to study combustion and evaporation of any single or multicomponent droplet. The water and acetone droplets were suspended from the quartz fiber using a syringe with a needle. The needle aided in controlling the droplet size. The initial mixtures were composed of 4:1 and 2:1 mass fraction of acetone and distilled water (Table 2.4).
Table 2.4: Compositions of water and acetone samples by volume Sample 1 2 Water (V, m ) 5e-6 5e-6
3
Acetone (V, m ) 1e-5 2e-5
The evaporation of these droplets was recorded with the Phantom IV (Vision Research, Wayne, NJ) high speed digital camera which captured images 20 frames per second. The Phantom IV high speed digital camera was attached with a K2 Long-Distance Microscope (Infinity Photo-Optical Company, Boulder, CO) for higher magnification (Fig. 2.1). The data for evaporation rate (i.e. diameter of the droplet as a function of time) of this mixture was obtained using the Vision Research image processing and analysis software compatible with the Phanton IV. The theoretical evaporation rate was calculated using equation 2.3.1: (2.3.1)
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where, kg is the equivalent thermal conductivity, l is the weighted density of water and acetone and, cpg is the specific heat of water and acetone mixture. The transfer number, Bq is is shown in Eq. 2.3.2.
(2.3.2)
where,
is the surrounding temperature, Ts is the temperature of the droplet
which is measured using a digital thermocouple thermometer and hfg is the heat of vaporization of the mixture. The experimental and theoretical values for evaporation rates for the two different compositions yielded an approximate 12% discrepancy (Table 2.5) likely attributed to estimates of thermal properties and droplet temperature.
Table 2.5: Comparison of theoretical and experimental evaporation rates of two different samples of water and acetone Sample KTHEORITICAL (mm2/s) KEXPERIMENTAL (mm2/s) % Discrepancy 11.8 10.4
1 2
-0.0034 -0.0080
-0.0030 -0.00717
KTHEORITICAL : Theoretical Burn rate KEXPERIMENTAL : Experimental Burn rate
After comparing the experimental and theoretical data for evaporation rates, it was concluded that the current apparatus can be used for droplet combustion.
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2.4. Testing procedure The Viton A and Al in acetone droplets were suspended from the quartz fiber using a syringe with a needle. The needle aided in controlling the droplet size. The solid-liquid mixture was injected onto the quartz fiber in form of small droplets, which travels roughly 1 cm vertically down the vertical fiber where the tiny droplets cumulates and suspends at the tip of the fiber. A 0.02 inch in diameter nichrome (Omega engineering, 80% nickel and 20% chromium) alloy wire of 10 mm in length and 30.4 /m resistance was bent and attached to the acrylic plate [19]. Using alligator clips, the nichrome wire was connected to the voltage source (Figure 2.5). The droplets were ignited by supplying 3 volts of AC current to the wire with a variac voltage transformer.
Heated Nichrome wire
Alligator clips
Figure 2.8: Heated nichrome wire
The evaporation and combustion of these droplets was recorded with the Phantom IV (Vision Research, Wayne, NJ) high speed digital camera
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which captured images 100 frames per second (Figure 2.3). The data for combustion rate (i.e. diameter of the droplet as a function of time) of this mixture was obtained using the Vision Research image processing and analysis software compatible with the Phantom IV.
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CHAPTER 3 RESULTS 3.1 Experimental Results Viton A (5%) burns with three distinct stages in an acetone droplet. The three stages are evaporation, combustion, and burning of residue with a distinct flame (Figure 3.1 & 3.2). During the first stage, the droplet evaporates until it steadily reaches the ignition temperature. The outer surface of the droplet evaporates with a gentle slope (Figure 3.3). Substantial vaporization occurs before the ignition takes place and ignition occurs only after the droplet is heated to an ignition temperature. The second stage begins with bubble formation inside the droplet and transitions into combustion. The combustion appears uniform throughout the droplet and has a steeper slope compared to the first stage (Figure 3.3). Figure 3.1 shows three consecutive still frame images taken during the transformation from evaporation to combustion. This third stage is the combustion of the remaining Viton A with a distinct flame (Figure 3.2).
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Figure 3.1: Still frame images of Viton-acetone droplet reaction dynamics: (a) Stage 1 evaporation; (b) transition from evaporation to combustion; (c) Stage 2 combustion.
Figure 3.2: Still frame images of 3rd Stage combustion of carbon residue resulting from
Viton-acetone droplet.
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1.5
Normalized diameter (mm/mm)
y = -0.2813x + 0.9889 R = 0.8669
Evaporation Combustion
0.5
Gentle Slope
Steep slope
y = -0.4515x + 0.9556 R = 0.9984
0 0 1 Time (s) (a) 1.5 2
Normalized Diameter (mm/mm)
y = -1.1293x + 1.0162 R = 0.981
0.5
0 0 0.5 Time (s) (b) Figure 3.3. Viton-acetone and nm-Al droplet regression rate for a) stage 1: evaporation and stage 2: combustion b) stage 3: secondary combustion. 1
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The bubble formation and subsequent combustion has been observed in the literature and described as disruptive burning of droplets [15]. Disruptive burning occurs when solid particles are added to a liquid droplet and the interior of a droplet reaches a nucleation temperature, which results in interior vapor generation and consequent rapid disruption of the liquid [15]. As the combustion progresses the droplet mass decreases and the droplet slowly regresses.
The rate of evaporation is negligible compared to the rate of combustion and thus ignored. The burn time is the time measured from the start of the combustion phase until the end of the reaction. The diameters and their corresponding times were recorded using the high speed camera compatible Phantom software (Figure 3.4).
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Dmax
Dmin
Figure 3.4: High Speed camera compatible Phantom software with diameter analysis
The concentration of nanometric Al (i.e., nm-Al) was doubled and then tripled. There is not a significant burn rate change when the amount of Al was increased but, there was behavioral change. The droplets with 5% or more nm-Al burns with a three-stage behavior. The burn rates are shown in Table 3.1. The support fiber geometrically distorts the shape of the burning droplet from spherical to ellipsoidal. Struk et. al report the different methods researchers typically present the equivalent diameter [17]. For comparison studies, only the Dmax was measured and normalized. Since, the current study
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is a comparison between burn rate and behavior of multicomponent droplets, the geometric distortion was neglected.
Table 3.1: The average burn rates and burn times for the droplets. Sample Avg. Burn Rate (mm/mm/s) Avg. Time 5% Viton
5% Viton +2.5% Al. (10-14 m)
5% Viton +2.5% Al. (80 nm)
-0.325+ 0.097 2.65 + 0.487
-0.0715 + 0.013 5.23 + 1.16
-0.393 + 0.089 2.13 + 0.318
Due to limitations of the current apparatus, it is not possible to control the initial diameter of the droplets.The burn rates shown in Table 3.1 are normalized by the largest diameter and presented in terms of mm/mm/s. For each test, this was done by dividing each diameter with the corresponding largest diameter from that test. This resulted in the maximum diameter of 1 for each test. The normalized diameter was then plotted with respect to time and the slope of the line is the burn rate. There is a significant difference in burn rate for the droplets containing nm-Al when compared to micron aluminum (i.e., micron-Al) even though they both show a two stage behavior. There is not a burn rate change with addition of nm-Al to the Viton-acetone droplets, but there is a distinct change in burning behavior. Viton and acetone shows a three stage burn behavior, whereas, nm-Al, Viton and acetone only shows a two stage behavior.
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Viton A (5%) in an acetone droplet with either 2.5% micron-Al (10-14 m) or in 2.5% nm-Al (80 nm) burns only with a two stage behavior (Figure 3.1). There was no burning of the excess residue observed in these droplets. A third stage was observed in acetone droplets with Viton A (5%) and 5% or more nm-Al. The third stage burning may occur from excess nm-Al and Viton A in a solid residue. To investigate this phenomenon further the second stage final diameter for each sample was measured. The sample with only Viton A has a higher amount of residue left after the second stage compared to the nm-Al in the Viton A droplet. This second stage droplet diameter may be related to the ignition of the third stage burning. Therefore, it can be concluded that the third stage may be the result from the unburned excess Viton A. A carbon residue is left after the combustion process). Addition of micron-Al to the Viton A and acetone droplet significantly decreases the burn rate whereas adding nm-Al almost doubles the burn rate. There is a significant difference in burn time between the droplets (Table 3.1).
3.2. Uncertainty Analysis The uncertainty associated with the measured burn rates and burn times is primarily controlled by random measurement error and droplet position for the different tests. The standard deviation was obtained using repeatability. Each multicomponent mixture was tested five times or more. The burn rate in Table 3.1 is an average of the burn rates from the different
26
tests. The standard deviation reported in Table 3.1 is based on the repeatability of the measurement.
27
CHAPTER 4 DISCUSSION One of the most interesting observations is the elimination of the 3 rdStage (burning of carbon reside) by the addition of Al to Viton-acetone droplets. The 2nd stage final droplet diameter for Viton-acetone droplets was observed to be double the 2nd stage droplet diameter for nm-Al-Viton-acetone droplet. This implies that the presence of Al may facilitate localized reaction sites that produce temperatures high enough to consume carbon from decomposing Viton (figure 4.2). Osborne et al. showed that fluorine from polythetrafluoroethylene (Teflon) bonds with Al particles and facilitates Teflon decomposition at reduced temperatures [21]. Further analysis revealed that fluorine actually bonds to vacant OH sites on the surface of alumina (Al 2O3) [22]. Aluminum particles are passivated with an alumina shell, and the specific surface area of the alumina shell has an effect on the onset of decomposition of the fluoropolymer (Teflon) [23]. As the specific surface area is increased, the onset of Teflon decomposition is reduced to lower temperatures [23]. In a similar way, fluorine from Viton may be attracted to Al particles and similarly catalyze the decomposition of Viton. Aluminum fluorination reaction (Al+F ) has an adiabatic flame temperature on the order of 4000 K [19]. These localized hot spots could react with carbon thereby reducing the amount of carbon residue available for 3rd-stage reaction. This effect is observed to be independent of Al particle size. However, the effect of Al particle size is clearly seen in the regression rate data from Fig. 4.1.
28
Regression Rate (mm/mm/s)
0.45 Micron Nano 0.3 Viton
0.15
0 0 2 4 Time (s) 6 8
Figure 4.1: Comparison of the regression rates
Figure 4.2: Droplets with Nm-Al particles
29
4.1. Simple Heat Transfer Model A simple heat transfer model for Viton and acetone droplets was established to predict the theoretical burn rate and transfer number. 4.1.1. Assumptions The following assumptions were made for this specific model: 1. Radial motion of the gasses is neglected therefore spherical geometry is assumed. 2. The transport properties are assumed to be independent of the radius of the droplet. 3. It is assumed that the droplet heats up to a steady temperature, therefore the thermal inertial of the droplet is negligible. 4. The adiabatic flame temperature was assumed as the flame temperature. 5. T is assumed the room temperature 25oC
4.1.2. Physical and Chemical Properties REAL code was used to determine the thermal conductivity, adiabatic flame temperature, heat of combustion [19]. REAL code is a chemical equilibrium modeling program designed for high temperatures and high pressures [19].
30
The calculations was made for reaction of 95% acetone with 5% in 33% of air2. The physical and chemical properties was used are 1. Temperature a. Flame Temperature [19]
b. Temperature of the Surface [20]
2. Average temperature: 751.82 K (4.1.2.1) 3. Specific Heat [21]
4. Thermal conductivity [19] (4.1.2.2) 5. Heat of Combustion [19]
6. Density [20]
7. Oxidizer-to-fuel ratio
Air is defined as N1.5618 O0.4190 Ar0.0093
31
4.1.3. Governing Equations The burning rate constant, K, was measured using Eq. 4.1.3.1. The D2 law for droplet burning is shown in Eq. 4.1.3.2. (4.1.3.1) (4.1.3.2) The flame temperature was calculated using Eq. 4.1.3.3. (4.1.3.3) The transfer number was calculated in MATLAB using Eq. 4.1.3.4. (4.1.3.4)
4.1.4. Discussion of the Dn model The transfer number predicted from the heat transfer model using MATLAB is
From Equation 1, the burning constant was calculated in MATLAB: mm2/s In conjunction with the theoretical burn rate constant, K, the experimental values for D, Do and t were used to determine n in Eq. (2). The values of n are shown in Table 4.1. The error was calculated based on the
32
assumption that for large droplets (i.e. droplets with D0 >1.18 mm [21]), the value of n = 1 [15].
Table 4.1. Determination of n power in the D Law for acetone-Viton droplets D0 (mm) 2.17 2.18 2.54 2.78 3.07 3.25 D (mm) 0.307 0.526 0.07 0.612 0.185 0.392 Time (s) 1.65 3.01 2.21 2.18 2.61 2.46 n 1.32 1.39 1.04 1.12 0.913 0.928 Error (%) 24.4 28.1 3.85 10.7 9.53 7.76
th n
Figure 4.3: The Transfer Number (B) as a function of the Burn Rate Constant (K) is represented.
Even though there are some differences in the burn rate, the heat transfer model can be used to estimate the burn rates for single or multicomponent droplets. Therefore, this simple heat transfer model can be
33
used to explain the experimental observations. The reaction can be described as a laminar diffusion mechanism. The occurrence of the third stage can be assumed a function of the droplet diameter after the second stage. To further investigate the occurrence of the third stage, a probabilistic analysis was developed for the Viton-Acetone and Viton, Acetone and nm-Al droplets. The probabilistic model predicts the occurrence of the third stage and is a useful tool that can be applied to combustion reactions to understand the reproducibility of a reaction phenomenon. The NESSUS software by Southwest Research Institute was used to perform the probabilistic analysis [18]. 4.2. Probabilistic Analysis NESSUS (Numerical Evaluation of Stochastic Structures Under Stress) combines probabilistic algorithms with general-purpose numerical analysis methods to compute the probabilistic response and reliability of engineered systems [18]. Analysis was performed to determine the following: 1. Probability that 3rd Stage will not occur for Viton -Acetone droplets, 2. Probability that 3rd Stage will not occur for Acetone-Viton -nAl droplets, 3. Probability of occurrence of the 3rd Stage for 2nd stage final droplet diameter of 0.5 mm. The following assumptions were made: 1. D2 and D3 are random variables (i.e. they are linearly independent).
34
2. 95% confidence level is enough to determine the goodness of fit 4.2.1. Determination of Probability Distribution A probabilistic analysis was performed using NESSUS software to determine the occurrence of the third stage in the multicomponent droplets. It was assumed that a 95% confidence level is necessary for the statistical tests. Kolmogorov-Smirnov (K-S) Test with 95% confidence level was performed on the droplets with and without the third stage. The assumed Cumulative Density function (CDF) of the theoretical distribution and the observed cumulative frequency were compared using the K-S test. The data was arranged in increasing order and then the maximum difference (D n) between the two CDF was estimated using equation 4.3.1 [13]. (4.3.1) where. FE(em) is the theoretical CDF of the assumed distribution at the mth observation of the ordered samples e m and Sm(en) is the corresponding stepwise CDF of the observed ordered samples [13]. (4.3.2) where m is the observation number and n is the sample size. The CDF of Dn (a random variable) can be related to the significance level as [13] (4.3.3) A standard mathematical table was used to obtain the at 95% significance
level [13]. According to the K-S test, of the maximum difference is less than or
35
equal to
, then the assumed distribution is acceptable at the significance
level of 95% [13]. The data points fitted the lognormal distribution slightly better than normal distribution (Table 4.1b, 4.2b). The mean, standard deviation, K-S Test data for both compositions are presented in table 4.1a,b & 4.2a,b. For the Viton and acetone droplets at significance level 95% and n = 5 the corresponding distribution is 0.563.For the Viton, nm-Al and acetone droplets at significance level 95% and n = 7 the corresponding distribution is 0.486. At significance level 95% and n <5, the corresponding distribution is Dn >0.563.
Table 4.2a: The normal and lognormal parameter for 3rd stage Viton/Acetone droplet initial diameter Normal Parameters 0.611 0.102 Lognormal Parameters = -0.504 = 0.175
Table 4.2b: The K-S Test parameters for 3rd stage Viton/Acetone droplet initial diameter FE(em ) m 1 2 3 4 5 Residue 0.467 0.548 0.650 0.673 0.717 Ln (residue) -0.762 -0.601 -0.431 -0.396 -0.333 Sn(en) 0.200 0.400 0.600 0.800 1.000 Normal 0.648 0.730 0.852 0.000 0.500 Lognormal 0.071 0.290 0.662 0.733 0.837 Normal 0.448 0.330 0.252 0.800 0.500 Dn Lognormal 0.129 0.110 0.062 0.067 0.163
36

nd
Table 4.3a: The normal and lognormal parameter for 2 stage Viton /Acetone droplet final diameter Normal Parameters 0.253 0.265 Lognormal Parameters = = -1.775 1.349
Table 4.3b: The K-S Test parameters for 2 stage Viton /Acetone droplet final diameter FE(em) m 1 2 Residue 0.065 0.440 Ln (residue) -2.729 -0.821 Sn(en) 0.500 1.000 Normal 0.240 0.760 Lognormal 0.240 0.760 Normal 0.260 0.240 Dn Lognormal 0.260 0.240
nd
4.2.2. Limit-State Function The reliability or probability of failure of the experimental data was evaluated using a specific performance criteria [13]. The mathematical representation of the limit state or performance function is defined below in equation 4.2.2.1 [13]. (4.2.2.1) where D2 is the residue diameter after 2nd stage for samples where third stage was not observed and D3 is the residue diameter after 2nd Stage for samples where third stage was observed. The failure surface or limit state of interest was defined as Z =1. D2 and D3 are assumed to be statistically independent random variables. Z >1 will imply the probability of the third stage not occurring. The nonoccurrence of the third stage in Viton and acetone droplets is considered a failure, and the occurrence of the third stage in nm-Al,
37
Viton and acetone are considered a failure. The information for probability of occurrence is obtained from the probability density function of random variables. Since the PDF of random variables was not available, an analytical approximation of the integral was performed using the first-order reliability method (FORM). The FORM method was used because it can be applied to both normal and lognormal variable. Due to the linear relationship between the random variables, the Second Order Reliability Method (SORM) is not necessary. 4.2.3. NESSUS Analysis and Results NESSUS, probabilistic design analysis software was used to perform the FORM analysis. The first order reliability method (FORM) with 95% confidence level was applied to compute the results. The CDF and PDF of the random variables generated by NESSUS are shown in figures 4.3 and 4.4. The value of Z0 was set to 1 because the distribution is lognormal.
Figure 4.4: CDF of Viton and Acetone droplets for 2nd stage final diameter a)without 3rd stage burning b) with 3rd stage burning
38
Figure 4.5: PDF of Viton and Acetone droplets for 2nd stage final diameter a)without 3rd stage burning b) with 3rd stage burning
Three set of analysis was performed in NESSUS. The first analysis set comprised of the combustion data from the Viton A and acetone droplets; and droplet diameter data from nm-Al, Viton A and acetone experiments. Figure 4.5 and 4.6 are the sensitivity analysis graphs. It was assumed that the initial third stage droplet diameter is same as the final diameter of the second stage. The second analysis set determined the probability of occurrence of the second stage final diameter of 0.5 mm for both compositions. The 2 nd stage final diameters were fitted into a normal distribution. The third set of analysis was performed to see the probability of having a final second stage droplet diameter of 0.5 mm for both compositions.
Table 4.4: The analytical results from NESSUS Composition Viton & Acetone
Test No. 1 (2 RVs) 2 (D2=0.5) 3 ( D2=0.5, all diameters) 1 (2 RVs) 2 (D2=0.5) 3 ( D2=0.5, all diameters)
Distribution Lognormal Normal Normal Lognormal Normal Lognormal
P(Z<0,1)* 0.921 0.871 0.516 0.0145 2.47E-07 .246
P(Z>0.1)* 0.0786 0.129 0.484 0.986 0.999 .703
Nm-Al, Viton & Acetone
39
*P(Z<0), P(Z>0) For normal variables *P(Z<1), (Z>0) For lognormal variables
Figure 4.6: the sensitivity graph for nm-al, Viton and acetone droplets for probability of occurrence of third stage combustion
Figure 4.7: the sensitivity graph for nm-al, Viton and acetone droplets for probability of occurrence of third stage combustion
40
4.2.4. Discussion of NESSUS Results The droplets of acetone with the fluoroelastomer, Viton A and either micron or nm-Al demonstrate a two or three stage behavior. A probabilistic analysis was conducted to determine the probability of observing the third stage for the different droplets. For Viton-Acetone droplets the probability of third stage occurring is 0.921 and the probability of third stage not occurring is 0.079. The sensitivity graphs indicate that D3 is more sensitive than D2. This shows that D3 has the most influence on the uncertainty of the response variable. The sensitivity factor indicates that for future data collection, priority should be given to D3. Also, the sensitivity graph indicates that sensitivity factors of the random variables are inversely relation. This is consistent with the limit-state function. The probability of occurrence third stage for the 2nd stage final diameter over 0.5 mm is 0.871. For nm-Al, Viton Acetone-Al droplets, the probability of 3rd stage occurring is 0.014 and probability of third stage not occurring 0.986. The probability of initial 3rd stage diameter of 0.5 is 0.703. Also, the probability of the occurrence of third stage for the 2nd stage final diameter of 0.5 mm is 2.4743E-07. Experimentally, it was observed that droplets of Viton and micron-Al do not show third stage even though the 2 nd stage final diameter is 0.6071+ 0.053 mm/mm/s. Since the residue from the droplets with micron-Al remain in
41
the third stage range and fail to show third stage burning, the micron maybe acting as a heat sink. The probabilistic analysis provided statistical data necessary to describe and predict burning behavior of multicomponent droplets and solidifies the argument for micron-Al acting as a heat sink in these liquid droplets.
42
CHAPTER 5 CONCLUSIONS The reaction dynamics of multicomponent droplets were investigated. The droplets of acetone with the fluoroelastomer, Viton A and either micron or nm-Al (2.5%) demonstrate a two stage combustion behavior. Droplets with only Viton A and acetone demonstrate a three stage behavior. The three stages are evaporation, combustion, and burning of excess product. The burn rate for droplets with micron-Al decreases 82% when compared to droplets with nm-Al. Droplet combustion was modeled as laminar diffusion and flame which resulted in a burn rate constant (k = 1.05 mm2/s) and n approximately 1. Probabilistic analysis was conducted to determine the probability of observing the third stage. The study predicted that Viton and Acetone has a high probability of demonstrating a third stage and nm-Al, Viton and acetone has a very low probability of showing a three stage behavior. Acetone droplets containing Viton and micron Al do not show a third stage possibly because micron Al is acting as a heat sink. Dissolving Viton A in acetone and adding Al is a technique that can be used to coat Al particles. Examining the combustion of the acetone-Viton-Al system has implications toward the safety and handling of this energetic material composite synthesis technique.
43
CHAPTER 6 SUGGESTED FUTURE WORK Compositions with equivalence ratio closer to 1 can be tested to see if there is any difference in the behavior of the droplets. Instead of acetone, other Viton solvents can be used and the same experiments can be repeated to further our understanding of these multicomponent droplets. For future work, more samples will be collected for the probabilistic analysis. This current sample size was too small to accurately determine the distribution for some of the parameters. A larger sample size will eliminate this problem and the K-S test can better determine the distribution. Priority should be given to D3 as indicated by the sensitivity graph.
44
REFERENCES [1] Dreizin, E.L., Aluminum Particle Ignition in Different Oxidizing Environments, (2009) article in press [2] Levitas, V.I., Asay, B.W., Son, S.F., Pantoya, M.L., Melt dispersion mechanism for fast reaction of nanothermites, Applied Physics Letters, published online 2006 Vol. 89. [3] Rai, A., Zhou, L., Prakash, A., McCormick, A., Zachariah, M.R., Understanding and tuning the reactivity of nano-energetic materials, Materials Research Society Symposium Proceedings, 2006, Vol. 896, pp. 99-110. [4] Pantoya, M.L., Granier, J.J., Combustion behavior of highly energetic thermites: Nano versus micron composites, Propellants, Explosives, Pyrotechnics, published online February 2005, Vol. 30, No. 1, pp. 53-62. [5] Levitas, V.I., Pantoya, M.L., Dikici, B., Melt dispersion versus diffusive oxidation mechanism for aluminum nanoparticles: Critical experiments and controlling parameters, Applied Physics Letters, published online 2008, Vol. 92, No. 1. [6] Rossi, C., Zhang, K., Estve, D., Alphonse, P., Tailhades, P., Vahlas, C., Nanoenergetic materials for MEMS: A review, Journal of Microelectromechanical Systems, published online, Vol. 16, No. 4, pp. 919-931. [7] Menon, L., Bhargava Ram, K., Patibandla, S., Richter, C., Sacco Jr., A., Ignition in Al-Fe2O3 nanocomposites, Materials Research Society Symposium Proceedings, published online 2005, Vol. 901, pp. 140-143; [8] Hohmann, Jr.BT., Vitons Impact on NASA Standard Initiaor Propellant Properties, NASA S-867, October 2000 [9 ] Glotov, O.G.,Yagodnikov, D.A., Vorob'ev, V.S., Zarko, V.E., Simonenko, V.N., Ignition, combustion, and agglomeration of encapsulated aluminum particles in a composite solid propellant. II. Experimental studies of agglomeration, Combustion, Explosion and Shock Waves, published online May 2007, Vol. 43, No. 3, pp. 320-333.
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[10] Kolarik, V., Juez-Lorenzo, M., Anchstegui, M., Fietzek, H., Multifunction high temperature coating system based on aluminium particle technology, Materials Science Forum, published online 2008, Vol. 595-598. PART 2, pp. 769-777. [11] Jouet, R.J., Carney, J.R., Granholm, R.H., Sandusky, H.W.. Warren, A.D., Preparation and reactivity analysis of novel perfluoroalkyl coated aluminium nanocomposites, Materials Science and Technology, published online April 2006, Vol. 22, No. 4, pp. 422-429. [12] Tsue, M., Kadota, T., Segawa, D., Yamasaki, H., Statistical analysis on onset of microexplosion for an emulsion droplet, Symposium (International) on Combustion, published online 1996, Vol. 1, pp. 16291635 . [13] Haldar, A., Mahadevan, S., Probability, Reliability and Statistical Methods in Engineering Design, 1st Ed., Wiley, 1999, pp. [14] Turns, Stephen N. Droplet Evaporation and Burning, An Introduction to Combustion: Concepts and Applications, 2nd Ed., McGraw-Hill, 1976, pp. 362-415. [15] Williams, F.A. Ignition and Burning of Single Liquid Droplets, Proceedings of the Thirty Fifth Congress of the International Astronautical Federation, AIAA Paris, France, 1984, pp. 547-553. [16] Bramley A, Brissaud D, Coutellier D, McMahon C,, Advances in Integrated Design and Manufacturing in Mechanical Engineering, 1st Ed., Springer, 2005, pp. [17] Struk, P.M., Ackerman, M., Nayagam, V., Dietrich, D.L., On calculating burning rates during fiber supported droplet combustion Microgravity Science and Technology, published online, 1998, Vol. 11, No. 4, pp. 144151. [18] B.H. Thacker, D.S. Riha, S.H.K. Fitch, L.J. Huyse, and J.B. Pleming, "Probabilistic Engineering Analysis Using the NESSUS Software," Structural Safety Structural Reliability Software, Vol. 28, No. 1-2, 2006, pp. 83-107. [19] Belov, B.V. (2004). REAL for windows, Moscow. [20] Mallinckrodt Baker Chemicals, http://www.jtbaker.com/ (Accessed November 19, 2009)
46
[21] Osborne, D.T., Pantoya, M.L., "Effect of Aluminum Particle Size on the Thermal Degradation of Al/Teflon Mixtures," Combustion Science Technology 2007, pp 14671480.
47
APPENDIX A ADDITIONAL GRAPHS OF ELLIPSOIDAL DIAMETER AS A FUNCTION OF TIME FROM A VITON A ACETONE EXPERIMENT.
3.5 3
y = -1.7339x + 2.843 R = 0.9452
D2ELL (mm2)
2.5
2 1.5 1 0.5 0 0 0.5 1 1.5 2
Time (s)
Figure A.1: (Test 1) Ellipsoidal diameter as a function of time
48
9 8 7 y = -3.1342x + 8.4311 R = 0.9244
D2ELL (mm2)
6
5 4 3 2 1 0 0 0.5 1
1.5
2.5
Time (s) Figure A.2: (Test 2) Ellipsoidal diameter as a function of time

8 7 6 D2ELL (mm2) 5 4 3 2 1 0 0 0.5 1 Time (s) 1.5 2 2.5 y = -3.0951x + 6.8705 R = 0.9822
49
9 8 7 y = -3.291x + 8.3953 R = 0.9746
D2ELL (mm2)
6
5 4 3 2 1 0 0 0.5 1
1.5
2.5
Time (s) Figure A.4: (Test 4) Ellipsoidal diameter as a function of time

6 5 4 3 2 1 0 0 0.5 1 1.5 2 2.5 3 3.5 y = -1.4412x + 4.9881 R = 0.8567
D2ELL (mm2)
Time (s)
50
APPENDIX B NORMALIZED DROPLET DIAMETER GRAPHS FOR VITON AND ACETONE

1.2 1 Diameter (mm/mm/s) 0.8 0.6 0.4 0.2 0 0 0.5 1 Time (s) 1.5 2 y = -0.525x + 0.979 R = 0.9866
Figure B.1: (Test 1) Normalized droplet diameter graphs for Viton and Acetone
1.2 1 Diameter (mm/mm/s) 0.8 0.6 y = -0.3709x + 1.1057 R = 0.9485
0.4
0.2 0 0 0.5 1 1.5 Time (s) 2 2.5 3
Figure B.2: (Test 2) Normalized droplet diameter graphs for Viton and Acetone
51
APPENDIX C ADDITIONAL NESSUS ANALYSIS DATA
Figure C.1: CDF of nm-al D2
Figure C.2: CDF of nm-al D3
52
Figure C.3: PDF of nm-al D2
Figure C.4: PDF of nm-al D3
53
APPENDIX D OUTPUT DATA FOR DIFFERENT TESTS
Limit State Value (Z0) = 1.0000 Standard Normal Variate (u) = 1.4145 Probability (Z<=Z0) = Probability u < 1.4145 = 0.9213875711 Probability (Z>Z0) = Probability u >= 1.4145 = 0.7861242894E-01 ************************************************************************ Most Probable Point Values printed by level ************************************************************************ ======================================================================== Level No. 1 Z = 1.00000 p = 0.921388 u = 1.414 Random Variable X MPP Std. Dev. from Mean u MPP -------------------------------------------------------------------------D2 0.577228 1.22518 1.39000 D3 0.577228 -0.332634 -0.261952 ************************************************************************ Probabilistic Sensitivity Results printed by level ************************************************************************ NOTE: FOR CORRELATED VARIABLES, THE FOLLOWING Alpha VALUES DO NOT CORRESPOND ONE-TO-ONE TO THE ORIGINAL RANDOM VARIABLES ======================================================================== Level No. 1 Beta = 1.414 Random Alpha d(beta)/ d(beta)/ d(prob)/ d(prob)/ Variable d(mean) d(std) d(mean) d(std) -------------------------------------------------------------------------D2 -0.9827 -3.064 -1.383 -0.4495 -0.2029 D3 0.1852 1.963 -0.7686 0.2880 -0.1128
Figure D.1: (TEST 1) NESSUS Analysis for Viton and Acetone droplets
54
Limit State Value (Z0) = 1.0000 Standard Normal Variate (u) = -2.1842 Probability (Z<=Z0) = Probability u < -2.1842 = 0.1447543838E-01 Probability (Z>Z0) = Probability u >= -2.1842 = 0.9855245616 ************************************************************************ Most Probable Point Values printed by level ************************************************************************ ======================================================================== Level No. 1 Z = 1.00000 p = 0.144754E-01 u = -2.184 Random Variable X MPP Std. Dev. from Mean u MPP -------------------------------------------------------------------------D2 0.619830 -0.364686 -0.346642 D3 0.619830 2.63289 2.15647 ************************************************************************ Probabilistic Sensitivity Results printed by level ************************************************************************ NOTE: FOR CORRELATED VARIABLES, THE FOLLOWING Alpha VALUES DO NOT CORRESPOND ONE-TO-ONE TO THE ORIGINAL RANDOM VARIABLES ======================================================================== Level No. 1 Beta = 2.184 Random Alpha d(beta)/ d(beta)/ d(prob)/ d(prob)/ Variable d(mean) d(std) d(mean) d(std) -------------------------------------------------------------------------D2 -0.1587 6.091 -2.342 -0.2237 0.8602E-01 D3 0.9873 -5.283 -18.39 0.1940 0.6753
Figure D.2: (TEST 1) NESSUS Analysis for Viton, nm-Al and Acetone droplets
55
Figure D.3: (TEST 2) NESSUS Analysis for the Viton and acetone droplet data
56
Figure D.4 (TEST 2) NESSUS Analysis for nm-Al, viton and acetone droplet data
57
Figure D.5: (TEST 3) NESSUS Analysis for the Viton and acetone droplet data
58
Figure D.6: (TEST 3) NESSUS Analysis for all nm-Al droplet diameter data
59
VALUES OF
Dn
APPENDIX E FOR THE KOLMOGOROV-SMIRNOV TEST
Figure E.1: Values of Dn for the Kolmogorov-Smirnov [13]
60

Sanjana Datta - Reaction Dynamics and Probability Study of Fluoroelastomer Coated Aluminum Particles Seeded in A Viton-Acetone Droplet

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Sanjana Datta - Reaction Dynamics and Probability Study of Fluoroelastomer Coated Aluminum Particles Seeded in A Viton-Acetone Droplet

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Reaction dynamics and probability study of fluoroelastomer coated aluminum particles seeded in a Viton-Acetone droplet

Fred Hartmeister Dean of the Graduate School

Copyright 2010, Sanjana Datta

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

4.1 4.2 4.3

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A.1 A.2 A.3 A.4 A.5 B.1

C.1 C.2 C.3 C.4 D.1 D.2

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Figure 2.1: SEM micrograph of Viton A

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Figure 2.2: Mass Scale

Texas Tech University, Sanjana Datta, May 2010

Table 2.2: Mass and Equivalence ratio for different compositions

1 Acetone Viton Aluminum1

2 10000 500 25 5262.5

3 10000 500 12.5 5256.25

4 10000 500 37.9196429 5268.95982

5 10000 500 0 5250 2.312

10000 500 12.5 5256.25

Figure 2.3 : a) Sonicator b) Sonicator tip

Composition 1,2, and 3 are nm-Al. 4 is micron aluminum composition.

Texas Tech University, Sanjana Datta, May 2010

Nm-Al (% mass)** 0 0 2.5 5.0 7.5

* Viton (%mass) = massviton/massacetone ** Al (%mass) = massAl/massviton

Figure 2.4: SEM micrograph of nm-Al particles (uncoated)

Texas Tech University, Sanjana Datta, May 2010

Figure 2.5: SEM micrograph of 2.5% nm-Al particles in Viton

Texas Tech University, Sanjana Datta, May 2010

Voltage Source Light Source

Droplet Suspension Apparatus

Figure 2.6: Experimental Set-up

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Screw at the bottom

Texas Tech University, Sanjana Datta, May 2010

Acetone (V, m ) 1e-5 2e-5

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is the surrounding temperature, Ts is the temperature of the droplet

KTHEORITICAL : Theoretical Burn rate KEXPERIMENTAL : Experimental Burn rate

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Heated Nichrome wire

Figure 2.8: Heated nichrome wire

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Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010

Texas Tech University, Sanjana Datta, May 2010