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Materials, Mechanical Characterization & ManufacturingMaterials, Mechanical Characterization &Manufacturing OverviewDavid R. Veazie, Ph.D. P.E., Professor and DirectorSouthern Polytechnic State UniversityCenter for Advanced Materials Research and Education - SPSUMaterials and Mechanical Testing Laboratories - CAUTest and Evaluation Research Opportunities WorkshopJuly 26 -28, 2012

Outline Material & Manufacturing Infrastructure Nanotechnology & Functional Materials Novel Nanoscale Characterization Equipment Full-Field Deformation and Structural Characterization AFOSR DURIP – Field Emission SEM Energetic Materials Advanced Material Development and Testing Novel Structural Testing and Implementation Advanced Power & Energy Generation Computational & Multi-Scale Modeling

Materials & Manufacturing InfrastructureEquipment and nter of excellence in composite manufacturingField Emission Scanning Electron MicroscopeAxial and axial-torsion servohydraulic test framesElevated temperature creep frames (composites)Ultrasonic NDI and environmental chambersMelt and capillary rheometry, extrusion and thermalimaging, compression molding, and thermoformingRTM, VARTM, autoclave, walk-in oven, 30T pressThermal analysis (TGA, DSC, TMA, DMA)Chemical analysis (NMR, FT-IR, Raman, Wet Lab)Microscopy (2 AFM's, TEM, X-Ray Diff)Vibrational and florescence spectroscopy

Materials & Manufacturing InfrastructureFaculty, Staff and Students (Last 3 Years)––––6 Faculty and 4 Full-Time Staff50 Supported Students (Engr. & Chemistry)18 Masters Graduates5 Ph.D. Graduates and 8 Ph.D. CandidatesProductivity (Last 6 Years)–––––––Over 100 Refereed Publications in Journals*Over 250 Conference Proceedings and Presentations3/4 of Publications Co-Authored by Students5 National Publication Student AwardsGenerated over 4 Million in External Research FundsOver 2.5 Million in Equipment PurchasedLab Maintains Upgrades & Calibrations* Some Government and Industry research restricts open literature publications

(AFOSR DURIP) Thermal Field Emission SEMVeazie (FA9550-11-1-0323) - Southern PolytechDr. David VeazieDr. Eric MintzA JOEL JSF-7600F Field Emission SEM wasinstalled in April 2012 at Southern Polytechnic StateUniversity. This SEM currently supports severalprojects including: Characterization of NanoparticleReinforced Resins for Readily Processable, HighSEM of separated graphene sheets with wrinklingTemperature, Low Density Composites (DoDW911NF-12-1-0084) and Characterization ofCopper Zinc Tin Sulfide (CZTS) for Photovoltaics(NSF 1125775).Copper Zinc Tin Sulfide (CZTS)thin films were prepared by anon-vacuum liquid-based coatingmethod enabling fabrication ofhigh-efficiency, low cost andtoxicity CZTS solar cell devices.A particle solution (slurry) wasdeveloped using the CZTSconstituents, varying the range ofcomposition ratios to achieve astable stoichiometric kesteriteCZTS crystal structure.Deidra HodgesSEM of 0.3 wt% graphite/PETI-298, clearlyconfirming the dispersed graphene.SEM of stoichiometric CZTS confirming theformation of a tetragonal crystal lattice structure.

Novel Materials & CharacterizationPrograms to Support Materials Research for Aerospace Industry Multiple programs investigating theprocessing and properties of nanocomposites Self Healing Composites Develop and characterize advancedcomposites which exhibit self-repairingproperties Thermal and mechanical analysis ofnano-structured thermoset polymers RTM composite process trials Georgia Research Alliance InnovationGrants Develop and deploy technologies thatlead to growing state’s economy LM Aero, AFRL and NASA sponsoreddevelopments

Nanotechnology & Functional MaterialsObjective Multiple programsinvestigating theprocessing andproperties of nanocomposites10000000eta* (P)G' (Pa)G'' 00Time (s)200025003000

Novel Nanoscale Characterization EquipmentMicro-Nano Test Frame (Patent-Pending)AFM Supporting PlateExchangeableLoad CellSampleMicro-translatorXY translationStageFigure 1: Schematic of AFM-MTS. a) with supporting plate; b) without supporting plate.Figure 5. AFM micrograph of electroplated Figure 6. AFM micrograph of electroplated5 hours(1.5x1.5 mm2 ).-Better load cell resolution (0.001 N at full scale) withultra-finerevolution)NiFe after annealedat 500 C forNiFe asdeposited (2x2loadmm2 ) stepping (1/1028-More accurate gripping of thin structures (No sample twisting)-Micro/Nanoscale strain measurement with AFM (Atomic Force Microscope)-Scan length: 100mm for use with microfabricated reference marks for nano-scale strain measurement-In-situ image monitoring of microstructure (characterize changes due to mechanical and thermal loading such as surfacemorphology, crack propagation, etc.

Advanced Material Development and TestingMetal Polymer Gap Filler Development-Successes on boot extrusion leads to study of innovative gap filler concept-Developed low cost, flexible and lightweight gap filler to replace conductive caulk-Highly successful IRAD sponsored program transitioned to production qualification-F/A-22 Door Edge Protection potential production supplier

Energetic Materials - AFRLRearrangingStrain Energyo Stiff particles in soft matrixo Different particle typeso Particle contacto Particle chainso Particle clustering1 2E dV2 V U111 2U dV E 2 dV or U dV2 V2 V2 V EIncluding Interparticle Friction Energy LossE 1 2dV2 V U DMA U FrictionU DMAU DMA 1 dV2 VAdapted from slide by B. White TMS 2010TestPreferenceOrder123456789105.0e 6DMA Measured StressDMADMA MeasuredMeasured StrainStrain0.0524.5e 6Strain (%)Stress (Pa)0.0504.0e 63.5e 63.0e 60.0480.0460.0442.5e 6Decreasing Volume Fraction0.042Decreasing Volume Fraction20%Al(50mm)mm)4mm)4mm)20%Al(5FV20%10% Al(5Ni 0 mm)(40mm) 20%10% Al(5Ni mm)(4mm)40%Al(5U Friction U Friction Friction Energy Particle * Tan Damping *40%Al(54mm)4mm)40%10% Al(5Ni 0 mm)(440%10% Al(5Ni mm)(40mm)mm)20%Al(54mm)20%Al(54mm)20%10% Al(5Ni 0 mm)(420%10% Al(5Ni mm)(440%Al(50mm)mm)40%Al(54mm)40%10% Al(5Ni 0 mm)(44mm)40%10% Al(5Ni mm)(42.0e 17.63242.94129.07258.118097.5Particles dFVTest Methodto MeasureElastic ModulusMiniature SHPBSHPBUltrasonic and VibratoryDynamic Mechanical AnalysisImpact and Taylor RodCompressionHardnessFlexureMiniature TensionTensionYoung's Modulus11Average DMA Measured Tangential Compliance-160mm)20%Al(5mm)20%Al(54mm)4mm)20%10% Al(5Ni 0 mm)(40mm)20%10% Al(5Ni mm)(4Decreasing Volume Fraction40%Al(50mm)20%Al(5mm)20%Al(54mm)4mm)20%10% Al(5Ni 0 mm)(40mm)20%10% Al(5Ni mm)(440%Al(5mm)40%Al(54mm)4mm)40%10% Al(5Ni 0 mm)(41 2dV2 V U DMA U Friction4Decreasing Volume Fraction40%10% Al(5Ni mm)(420%Al(50mm)mm)Al(520%4mm)20%10% Al(5Ni 0 mm)(44mm)20%10% Al(5Ni mm)(440%Al(50mm)mm)Al(540%4mm)4mm)E mm)54.0e 53.0e 540%10% Al(5Ni 0 mm)(4740%Al(50.05.0e 584mm)DecreasingVolume Fraction5.0e-76.0e 59 1 34mm)1.0e-6d T 1 dT 4a mN 40%10% Al(5Ni 0 mm)(41.5e-6(Averaged over Particle Volume Fractions, Vf)7.0e 5DMA DataDMA Friction ModelCompression Data10E (GPa)2.0e-640%10% Al(5Ni mm)(4Friction Energy (N-m)2.5e-6Tangential Stiffness T d (Pa)240%10% Al(5Ni mm)(4Particle Friction Energy53239 mP T 5 T1 T1 1 1 1 E 1 1 10a mP 6 mP mP 3.0e-6

Advanced Power & Energy GenerationMicro-Gas Turbine EnginePower MEMS Technology

Computational & Multi-Scale ModelingObjective Develop multi-scale technologyto link molecular scale tostructural cale ModelMeso-scale RandomnessStochastic omputationalStructural MechanicsCompositeStructuralMechanics

Full-Field Structural CharacterizationFull-Field Deformation Measurement with DigitalCorrelations Software (Optical Strain)(a) Wrinkle Coupon Test Setup(a) Short Beam Shear Test Setup(c) Transverse Normal Strain Contour Plot(c) Transverse Normal Strain Contour Plot(b) Axial Strain Contour Plot(d) Shear Strain Contour Plot0.2”SupportSupport0.4” (10.2 mm)(b) Axial Strain Contour PlotDelamination about to initiate(d) Shear Strain Contour Plot-Stereo Camera Set for Capturing 3D Surface Shape and Full-Field Deformation-Optical Strain from Digital Correlations Software(a)(b)Impact Surface Shape for (a) Front and (b) Back Surfaces

Novel Structural Testing and ImplementationC-130J Emergency Exit Door Structural Qualification Tests-Structural validation testing of high speed machined monolithic door design-Static and fatigue pressure testing conducted in Mechanical Test Lab-Developed test set-up, strain monitoring and data acquisition system-FAA Certified (C-130J implementing new design)

Aerospace Materials – Lockheed-MartinF/A-22 Material ScreeningUltimate Bearing Strength , FBTu200000190000180000Room Temperature170000-65 Fpsi Screen 6 commercially available RTM epoxiesfor F/A-22 qualification Industry standards for damage tolerance, OHC,bearing and T-elements Scope of effort Build flat and element tooling Fabricate 28 flat panels Fabricate 14 T-elements Coupon/element machining Moisture conditioning Mechanical Test NDI Dynamic mechanical analysis Photomicroscopy Program completed in 7 months220 F160000220 F Wet150000140000130000RTM 6LoctiteNBR77CycomMaterialRS50VR 65250-4

Aerospace Materials – Lockheed-MartinHigh Temperature Polyimides VARTM of NASA PETI resins Process temperatures up to 700 F using hightemperature injector Scope of effort Resin rheology 6 glass and carbon panels NDI Developed process which achieved 4% voidcontents (typical of VARTM) Demonstrated comparable hightemperature properties between VARTMand RTM Related programs with engine andspacecraft contractors

Aerospace Materials – Lockheed-MartinF/A-22 Door Edge Protection Replacing labor intensive injectionmolding of “boots” with extrusion Continuous extrusion of boot and sheetpermits fabrication of entire productionlots in hours (vs. weeks) Efforts conducted using Haake R&Dextruder Scope of Aero efforts Screening nylons and urethanes Optimize filler loading fractions Extrusion tooling Thermal analysis/physical testing Highly successful IRAD sponsoredprogram transitioned to productionqualificationLoadings B,C, DLoading ABaseline

Aerospace Materials – Lockheed-MartinP-3 Orion Fairing Fabrication Develop, build, and certify low costcomposite components for P-3 aircraft Replaces corrosion sensitive componentson aging aircraft platform with VARTMcomposites First effort within LM Aero to buildflight worthy hardware for manned A/C Selected component – Aft lower wingfillet panel Scope of effort Full scale tooling Design property testing Sub and full scale fabrication Program completed in 12 months

Aerospace Materials – Lockheed-MartinP-3 Orion Test Article Fabrication Fabrication efforts performed in new compositeslaboratory Efforts performed Built 9 design property panels Built 8 subcomponent articles Built 2 full scale articles Coupon machining Moisture conditioning Mechanical testing NDI Laminate physical testing Dynamic mechanical analysis Photomicroscopy Very successful part replacement studyperformed from “cradle to grave”

Aerospace Materials – NASA LaRCReusable Launch Vehicle (RLV) Program500Flatwise Tensile StrengthTensile Strength (Psi)Objective Verify LaRC polyimide foam materials reliabilityfor vehicle lifetime Standards for Thermal Protection System,Support Structure and Cryogenic fuel tanksScope of effort Test and characterize mechanical/thermalmaterial properties Develop predictive methods and processingparameters Fabricate and characterize sandwich compositesAccomplishments Novel fabrication methods characterized Cost reduction in foams Fabricate flame resistant panels400RTA300 F-65 F30020010000.5 pcf2 pcf5 pcfFoam Material8 pcf