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Thermal
 

Thermal

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    Thermal Thermal Presentation Transcript

    • Materials Characterization Lab www.mri.psu.edu/mcl Thermal Analysis R.I. Malek Materials Characterization Laboratory University Park, PA 16802
    • Materials Characterization Lab www.mri.psu.edu/mcl Personnel • Raafat Malek, Director • Magda Salama, Mass Spec, Thermal analysis. • Tim Klinger, Mass Spec.
    • Materials Characterization Lab www.mri.psu.edu/mcl Outline • Definition • Uses • Information Provided • Techniques • TGA, • DTA, DSC, SDT, • TMA, DMA •Thermal Expansion, Diffusivity • Instruments • Some Applications • Reaction Kinetics •New Instruments
    • Materials Characterization Lab www.mri.psu.edu/mcl Definition Thermal Analysis is a series of techniques that measure materials properties as a function of temperature, time and atmosphere.
    • Materials Characterization Lab www.mri.psu.edu/mcl Uses Research and Development: • Development and selection of new materials, • Performance and evaluation of existing materials. Quality Control: • Fingerprinting, • Monitoring and certification. • Troubleshooting.
    • Materials Characterization Lab www.mri.psu.edu/mcl Information Provided • Melting Point, • Glass Transition, • Crystallinity, • Curing and Cross-Linking, • Heat Capacity, • Stability, • Purity, • Composition, • Modulus of Expansion, • Reaction Kinetics.
    • Materials Characterization Lab www.mri.psu.edu/mcl Techniques
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl Instruments at MRL TGA/MASS SPECTROMETER
    • Materials Characterization Lab www.mri.psu.edu/mcl Balance Purge in Furnace Purge exit Furnace Purge in
    • Materials Characterization Lab www.mri.psu.edu/mcl New Mass Spectrometer
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl Some Applications Percent Amorphous Carbon Left over During Nano Carbon Synthesis Sample: AP8256R/365/90 File: C:...8256R36590.001 TGA-DTA Size: 6.2373 mg Operator: Clascidia Run Date: 18-Nov-02 15:18 Comment: 5C/min up to 800C in air 110 0.6 TGA/DTA Determining the Percent of Amorphous Carbon in Carbon Nano Tubes Carbon Nano Tubes 100 0.4 Temperature Difference (°C/mg) Amorphous Carbon 90 0.2 Weight (%) 80 0.0 70 -0.2 60 -0.4 0 200 400 600 800 Exo Up Universal V2.6D TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl Reduction of Ferric Oxide by a Mixture of CO + CO2 Sample: Ferric Oxide File: C:...Ferric Oxide.001 TGA Size: 28.8550 mg Operator: Malek Run Date: 15-Oct-02 10:13 Comment: Purge with CO-CO2 102 TGA Ferric Oxide 100 3.515% 98 (1.014mg) Weight (%) 96 94 4.719% (1.362mg) 92 90 0 200 400 600 800 1000 Universal V2.6D TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl Thermal Decomposition of Gypsum in a Hermetic pan Sample: Gypsum hermetic File: C:...New DataGypsum H DSC Size: 4.9000 mg Operator: Magda Method: Magda1.myth Run Date: 21-Jul-00 10:02 1 DSC Decomposition of Gypsum in a Hermetic Pan 179.37°C 97.05J/g 0 135.45°C 281.5J/g Heat Flow (W/g) 193.26°C -1 Hemihydrate -----> Anhydrous (0.5 Molecules of Water Lost) -2 -3 146.64°C Dihydrate -----> Hemihydrate (1.5 Molecules of Water Lost) -4 0 50 100 150 200 250 300 Exo Up Universal V2.6D TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl Reaction of Liquid Crystal and PMMA
    • Materials Characterization Lab www.mri.psu.edu/mcl New Rocket Fuel from Nano Aluminum Powder Sample: Nano Al Powder for Rocket Fuel File: C:...OxygenNanotech-1.001 DSC-TGA Size: 3.4587 mg Operator: Malek Run Date: 1-Nov-02 08:50 Comment: Oxygenn Purge 160 10 549.12°C 140 0 Heat Flow (W/g) 53.45% (2Al --------> Al2O3) 519.20°C Weight (%) (1.849mg) 6723.J/g 120 -10 100 -20 80 -30 200 400 600 800 1000 Exo Up Universal V2.6D TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl Barium Titanate System Sample: 72 Air 1200 File: D:72a1200_pw_1.003 DSC Size: 12.1000 mg Operator: Filimonov Method: BaTiO3 Run Date: 13-Feb-02 16:17 Comment: s72 1.01BaO*TiO2 Air A3_49 1200c powder/Pt Instrument: 2920 DSC V2.4F 0.3 123.00°C 0.2 124.40°C 0.6033J/g Heat Flow (W/g) 0.1 123.82°C 0.6213J/g 0.0 127.89°C -0.1 0 50 100 150 200 Exo Up Universal V3.3B TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl Reaction Kinetics Arrheneus Equation K = A exp(-Ea /RT) K = Reaction Rate A= Constant Ea= Activation Energy R= Gas Constant T= Temperature
    • Materials Characterization Lab www.mri.psu.edu/mcl
    • Materials Characterization Lab www.mri.psu.edu/mcl Decomposition of Calcium Oxalate at different heating rates Third weight loss 70 60 Weight (%) 5C/min 10C/min 1C/min 0.05C/min 0.1C/min 50 40 30 500 550 600 650 700 750 Universal V2.6D TA Instruments Temperature (°C)
    • Materials Characterization Lab www.mri.psu.edu/mcl TGA/MASS SPEC of Carbon
    • Materials Characterization Lab www.mri.psu.edu/mcl TGA/MASS SPEC OF NEW CARBON FUEL 30 ––––––– Mass Spec/ Magda 100 m/e 44 TGA 25 m/e 41 20 80 m/e 43 Ion Current (nA) Weight (%) 15 m/e 15 CO2 10 60 C3H7 CxHy 5 CH3 m/e 2 H2 C2H6 m/e 30 40 0 0 100 200 300 400 500 600 Temperature (°C) Universal V4.1D TA Instruments
    • Materials Characterization Lab www.mri.psu.edu/mcl Thermal Characterization is available according to International Standards: Technique Industrial Standards DSC, DTA ASTM C 351, D 3417, D 3418, D 3895, D 4565, E 793, E 794 DIN 51004, 51007, 53765, 65467 DIN EN 728 ISO 10837, 11357, 11409 Pressure DSC ASTM D 5483, D 6186, E 1782, E 1858, E 2009 TGA & STA (TGA-DSC/DTA) ASTM E 914, E 1131, E 1868 w. MS & FTIR / evolved gas analysis DIN 51006 ISO 7111, 11358 DIL/TMA ASTM D 696, E 228, E 831, E 1363, E 1545, E 1824 Thermal Expansion & Sintering DIN 53752 DMA ASTM D 4092, D 4065, D 4473, D 5023, D 5024, D 5026, D 5418, E 1640, E 1867 DIN 53440 DIN EN ISO 6721 DEA Dielectric Analysis ASTM E 2038, E 2039 Thermal Conductivity ASTM C 177, C 236, C 518, C 335, C 976, D 5470, E 1225, E 1530, F 433 ISO 8301, 8302 Flash / Thermal Diffusivity ASTM E 1461 DIN 30905 DIN EN 821
    • Materials Characterization Lab www.mri.psu.edu/mcl Thermal Analysis Books • MACKENZIE, Differential Thermal Analysis, 1970 Vol. I Fundamentals Vol. II Instrumentation and Techniques. • Several books on specific materials. • Thermal Analysis journals. • North American Thermal Analysis Society (NATAS)
    • Materials Characterization Lab www.mri.psu.edu/mcl Acceptable sample forms: Solids Powders Liquids
    • Materials Characterization Lab www.mri.psu.edu/mcl Gases used for regular thermal analysis: Dry Air. Nitrogen. Argon. Mix 40% Carbon Monoxide + 60% Carbon Dioxide. Mix 5% Hydrogen + 95% Nitrogen or Argon. Gases used for TGA/Mass Spec analysis: Extra High Purity Argon or Nitrogen.
    • Materials Characterization Lab www.mri.psu.edu/mcl New Instruments ASAP 2020 Accelerated Surface Area and Porosimetery Analyzer. Unique Capability • Two Independent vacuum systems. • Oil-free “dry” vacuum pump. • Intelligent degas system. • New long-duration cryogen system. • Automated selection of gas • Ability to connect to a mass spec.
    • Materials Characterization Lab www.mri.psu.edu/mcl Ranges of pore sizes and techniques
    • Materials Characterization Lab www.mri.psu.edu/mcl Adsorption of gas on surface of solid 4 3 2 1
    • Materials Characterization Lab www.mri.psu.edu/mcl Adsorption Desorption Isotherm Isotherm Linear Plot (LICHRSP1) - Adsorption (LICHRSP1) - Desorption 40 35 30 Quantity Adsorbed (cm³/g STP) 25 20 15 10 5 0 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00 Relative Pressure (p/p°)
    • Materials Characterization Lab www.mri.psu.edu/mcl ASAP 2020 Chemisorption Option Uses the static volumetric technique to determine the percent metal dispersion, active metal surface area, size of active particles, and surface acidity of catalyst materials.
    • Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920
    • Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920 • Fully automated catalyst characterization. • Probing active sites On catalyst surface.
    • Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920 • Adsorption – Pulse Chemisorption • Temperature Programmed Studies – TPR – TPD – TPO
    • Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920 Residual Gas Analysis • TCD - all gases TCD • Mass Spectrometer 100 200 300 400 – i-Propylamine (iPA) – Ammonia (NH3) iPA – Propylene (C3=) 100 200 300 400 NH3 • RGA confirms decomposition of iPA 100 200 300 400 C3= 100 200 300 400
    • Materials Characterization Lab www.mri.psu.edu/mcl Thermal Analysis Charges • Instrument Charge = $30/Sample. • Training, data interpretation, sample set-up, etc) = $30/hr. • Consultation time to discuss your samples, data, etc is free.
    • Materials Characterization Lab www.mri.psu.edu/mcl Campus resources- people • Raafat Malek, 109 Materials Research Lab Building, Hastings Road 865-7341 rqm@psu.edu • Jeff Shallenberger, 196 MRI Bldg 865-0337 jxs124@psu.edu Other resources: • www,mri.psu.edu/mcl/techniques/thermal.asp (links, applications, etc) • MRI links to publications and abstract (Web of Science) searching (www.mri.psu.edu/linkspubs/) • The Libraries (http://www.lias.psu.edu/)