1. Rheological Capabilities at TACOM-ARDEC
Presented by:
Leslie Fishbein
Armament Systems Process Division
WECAC

2. Purpose
Provide an overview of efforts to establish a state-of-the-art energetic materials characterization laboratory at TACOM-ARDEC

3. Outline
Mission
Equipment Capabilities
Future Work
Summary

4. The TACOM-ARDEC Mission
The Rheology Laboratory will enhance TACOM-ARDEC’s role as a leading developer of new energetic compositions and processes:
FCS propellants in support of the Multi-role Armament and Ammunition System (MRAAS)
State-of-the-art processing of energetic materials at the Building 1403 Twin-Screw Mixer/Extruder
Process modeling and simulation
Support of items in production (e.g., M30A1, JA-2, AA-2, PAP-7993, M14, Ball Powders)
Opportunities to team with Industry and Academia:
Stevens Institute of Technology (SIT)
Polymer Processing Institute, New Jersey Institute of Technology (NJIT)
ATK/Radford AAP
GENCORP Aerojet
ATK/Thiokol Propulsion

5. The Rheological Laboratory
Consolidate rheological capabilities under one roof:
Remotely operated systems
User friendly software for data acquisition and analysis
Support TACOM-ARDEC material characterizations:
Energetic materials (Propellants, Explosives, Pyrotechnics)
Precursor Materials (e.g., ETPEs, binders)
Plastics
Epoxies
Composites
Resins
Support process modeling and simulation efforts:
Twin-Screw Mixer/Extruder
Shear Roll Mill
Cryogenic Polymerization Reactor

6. Capillary Rheometer
Similar to laboratory-scale extruder that is highly instrumented and accurately controlled
Relate changes in processing conditions (pressure, temperature) of extrusion to product properties (mechanical, ballistic)
Characterize the rheological/flow properties of energetic materials under different conditions (temperature, composition)
Obtain a constitutive equation for the energetic materials for process analysis and simulation using RheoPlotter software
Instron Load Frame Model #5581 and
Shear Tool Capillary Adapter Assembly

7. Capillary Rheometer
To determine the rheological properties as a function of shear rate, temperature, pressure, and molecular weight, which is crucial to the design and control of process operation
Apply Different Speeds (S) at controlled Temperature
Reservoir
Capillary
Plunger S ~
Obtain Forces (Resistance to Flow)
Data Analysis
Viscosity = F (shear rate, temperature)
Relate To
Die Forming
Flow in Processing Equipment

8. Rheometric Scientific Dynamic Analyzer- RDA III
Rotational Rheometer
Study the dynamic mechanical properties of the energetic materials (G, G, tan )
Study the complex viscosity (*) and viscoelastic behavior
Investigate the molecular structure and interaction/compatibility between the ingredients of the energetic materials
Study the reaction kinetics of reactive system
Rheometric Scientific Dynamic Analyzer- RDA III

9. Rotational Rheometer Measures viscosity, elasticity and shear modulus
Can perform controlled strain, stress and strain rate experiments
Includes range of test fixtures:
Parallel plate
Torsion fixtures
Allows for characterization from:
Suspensions, emulsions,
Polymer melts, elastomers
Solids
Apply Strain A=A0sint where A0: small amplitude
Measure Torque, Normal Force
Obtain Normal Force, Torque Torque = T sin t + T cos t
Data Analysis
Elastic Properties
Viscous Properties
Apply Strain A=A0sint
Relate To
“Structure” of the Mixture (MW, concentration, degree of mixing, compatibility, crosslinking)

10. Torque Rheometer
The Poly Lab 300p enables production of small batches with simultaneous recording of torque and time while mixing material:
High torque capability
Oil heated and cooled chamber and plates
Rotors for different shear ranges:
Roller blades (viscous properties for thermoplastics & thermosets)
Cam blades (thermoplasts & elastomers in medium shearing range)
Banbury blades (natural and synthetic rubber)
Sigma blades (low shear ranges; most suitable f/energetic materials)
Teflon bushings to test chemically aggressive media
Special tools to clean the mixer parts
Pneumatic ram
Poly View data evaluation; i.e.:
Routine evaluation --Rheograms (torque vs. time)
Multi curve Analysis

11. Thermo Haake Poly-Lab 300p System
Torque Rheometer
The torque rheometer is capable of the measuring the following:
Dynamic viscosity depending on shear load
Melt behavior in the extruder
The influence of additives
Temperature and shear load behavior
TACOM-ARDEC will mainly be using Rheometer for it’s mixing capabilities
Thermo Haake Poly-Lab 300p System

12. Internal Mixer Torque Rheometer
Apply rpm () = Constant at Controlled Temperature
Obtain Torque (time)
Data Analysis
Specific Energy Requirement for Mixing, Reaction = F (time)
Relate To
Mixing, Reaction = F (axial distance) in an extruder

13. Planned Work Loading – FY 03
Army
Characterization of JA-2 and AA-2 propellant produced on a Shear Roll Mill (ManTech)
Supports modeling activity w/SIT
Leveraged with implementation of SRM technology in support of the manufacture of solventless propellants at Radford AAP
Characterization of ETPEs (ManTech)
Supports TACOM-ARDEC modeling activity and ETPE process optimization
Begin developing of rheological data base for energetic materials consider for TSE processing (ManTech)
Propellants (e.g., M39 / M43 LOVA)
Explosives (e.g., PAX-2A IM)
Pyrotechnics (e.g, M206, MJU-7A/B, MJU-53/B)
155-mm M485 Illumination Round
Characterization of replacement material for liquid polysulfide

14. Planned Work Loading Initiatives
Potential (3rd party)
ATK / Radford AAP (gun propellants):
Full-time PhD Rheologist -- no laboratory capability
ATK / Thiokol Propulsion (rocket and gun propellants)
GENCORP Aerojet (CRADA tasking)
BAE Systems / Holston AAP (explosives)
SIT (in support of process modeling)
PPI, NJIT (CRADA):
Expand PPI commercial market place through use of Rheology Laboratory at TACOM-ARDEC

15. Summary Rheology Lab is in full operational status
The characterization of Energetics is to be used to understand, simulate, design, and optimize the manufacturing processes
CRADA has been signed with PPI/NJIT
Future work is being discussed with SIT, ATK, and Aerojet
Questions and Inquires to be addressed to:
Lilia Mastov
TACOM-ARDEC
(973)