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Materials Characterization Lab
                                    www.mri.psu.edu/mcl




     Thermal Analysis

        ...
Materials Characterization Lab
                                         www.mri.psu.edu/mcl




                 Personnel...
Materials Characterization Lab
                                         www.mri.psu.edu/mcl

                         Outl...
Materials Characterization Lab
                                   www.mri.psu.edu/mcl




Definition

Thermal Analysis is ...
Materials Characterization Lab
                                           www.mri.psu.edu/mcl




Uses
Research and Develo...
Materials Characterization Lab
                                  www.mri.psu.edu/mcl



Information Provided
• Melting Poi...
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 SPECTR...
Materials Characterization Lab
                                  www.mri.psu.edu/mcl


Balance Purge in




Furnace
Purge
...
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
                                                                                           ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                          www.mri.psu.edu/mcl



Reaction of Liquid Crystal...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                       www.mri.psu.edu/mcl




              Reaction Kinet...
Materials Characterization Lab
    www.mri.psu.edu/mcl
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                              www.mri.psu.edu/mcl


TGA/MASS SPEC of Carbon
Materials Characterization Lab
                                                                                  www.mri.p...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                                        www.mri.psu.edu/mcl




           ...
Materials Characterization Lab
                               www.mri.psu.edu/mcl




Acceptable sample forms:

          ...
Materials Characterization Lab
                                               www.mri.psu.edu/mcl




Gases used for regul...
Materials Characterization Lab
                                                   www.mri.psu.edu/mcl

New Instruments
ASA...
Materials Characterization Lab
                                      www.mri.psu.edu/mcl




Ranges of pore sizes and tech...
Materials Characterization Lab
                                                www.mri.psu.edu/mcl


Adsorption of gas on ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                     www.mri.psu.edu/mcl

ASAP 2020 Chemisorption Option


...
Materials Characterization Lab
                       www.mri.psu.edu/mcl



AutoChem II 2920
Materials Characterization Lab
                                www.mri.psu.edu/mcl



             AutoChem II 2920


• Fu...
Materials Characterization Lab
                             www.mri.psu.edu/mcl




          AutoChem II 2920

• Adsorpti...
Materials Characterization Lab
                                           www.mri.psu.edu/mcl




              AutoChem I...
Materials Characterization Lab
                                                www.mri.psu.edu/mcl




Thermal Analysis Ch...
Materials Characterization Lab
                                                                 www.mri.psu.edu/mcl




Ca...
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Thermal

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Transcript of "Thermal"

  1. 1. Materials Characterization Lab www.mri.psu.edu/mcl Thermal Analysis R.I. Malek Materials Characterization Laboratory University Park, PA 16802
  2. 2. Materials Characterization Lab www.mri.psu.edu/mcl Personnel • Raafat Malek, Director • Magda Salama, Mass Spec, Thermal analysis. • Tim Klinger, Mass Spec.
  3. 3. 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
  4. 4. 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.
  5. 5. 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.
  6. 6. 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.
  7. 7. Materials Characterization Lab www.mri.psu.edu/mcl Techniques
  8. 8. Materials Characterization Lab www.mri.psu.edu/mcl
  9. 9. Materials Characterization Lab www.mri.psu.edu/mcl
  10. 10. Materials Characterization Lab www.mri.psu.edu/mcl
  11. 11. Materials Characterization Lab www.mri.psu.edu/mcl
  12. 12. Materials Characterization Lab www.mri.psu.edu/mcl Instruments at MRL TGA/MASS SPECTROMETER
  13. 13. Materials Characterization Lab www.mri.psu.edu/mcl Balance Purge in Furnace Purge exit Furnace Purge in
  14. 14. Materials Characterization Lab www.mri.psu.edu/mcl New Mass Spectrometer
  15. 15. Materials Characterization Lab www.mri.psu.edu/mcl
  16. 16. Materials Characterization Lab www.mri.psu.edu/mcl
  17. 17. 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)
  18. 18. 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)
  19. 19. 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)
  20. 20. Materials Characterization Lab www.mri.psu.edu/mcl Reaction of Liquid Crystal and PMMA
  21. 21. 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)
  22. 22. 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)
  23. 23. 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
  24. 24. Materials Characterization Lab www.mri.psu.edu/mcl
  25. 25. 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)
  26. 26. Materials Characterization Lab www.mri.psu.edu/mcl TGA/MASS SPEC of Carbon
  27. 27. 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
  28. 28. 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
  29. 29. 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)
  30. 30. Materials Characterization Lab www.mri.psu.edu/mcl Acceptable sample forms: Solids Powders Liquids
  31. 31. 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.
  32. 32. 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.
  33. 33. Materials Characterization Lab www.mri.psu.edu/mcl Ranges of pore sizes and techniques
  34. 34. Materials Characterization Lab www.mri.psu.edu/mcl Adsorption of gas on surface of solid 4 3 2 1
  35. 35. 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°)
  36. 36. 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.
  37. 37. Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920
  38. 38. Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920 • Fully automated catalyst characterization. • Probing active sites On catalyst surface.
  39. 39. Materials Characterization Lab www.mri.psu.edu/mcl AutoChem II 2920 • Adsorption – Pulse Chemisorption • Temperature Programmed Studies – TPR – TPD – TPO
  40. 40. 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
  41. 41. 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.
  42. 42. 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/)
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