1. Vielitzer Straße 43 95100 Selb GERMANY Tel.:0049 9287 8800 Fax:0049 9287 70488 Email: info@linseis.de Linseis Inc. 20 Washington Road P.O.Box 666 Princeton-Jct. NJ 08550 Tel.:(609) 799-6282 Fax:(609) 799-7739 Email: info@linseis.com

2. The Company Since 1957 Linseis Corporation delivers outstanding service, know how and leading innovative products in the field of thermal analysis and thermal physical properties. We are driven by innovation and customer satisfaction. Customer orientation, innovation, flexibility and last but not least highest quality are what Linseis stands for from the very beginning. Thanks to these fundamentals our company enjoys an exceptional reputation among the leading scientific and industrial companies. Claus Linseis Managing Director

3. ASTM E 1461 - 01 Standard Test Method for Thermal Diffusivity by the Flash Method A small, thin disc specimen is subjected to a high intensity short duration radiant energy pulse. The energy of the pulse is absorbed on the front surface of the specimen and the resulting rear face temperature rise (thermogram) is recorded. The thermal diffusivity value is calculated from the specimen thickness and the time required for the rear face temperature rise to reach certain percentages of its maximum value. When the thermal diffusivity of the sample is to be determined over a temperature range, the measurement must be repeated at each temperature of interest.

4. Terminology 1 Definitions of Terms Specific to This Standard: 1.1 thermal conductivity, l, of a solid material—the time rate of steady heat flow through unit thickness of an infinite slab of a homogeneous material in a direction perpendicular to the surface, induced by unit temperature difference. The property must be identified with a specific mean temperature, since it varies with temperature. 1.2 thermal diffusivity, a, of a solid material—the property given by the thermal conductivity divided by the product of the density and heat capacity per unit mass.

5. Classification of some Thermophysical Properties Thermophysical Properties Thermodynamic Properties Transport Properties Thermal Diffusivity LFA Specific Heat DSC Thermal Expansion Dilatometer Thermal Conductivity Mass Diffusion Coefficient Electric Resistivity Kinematic Viscosity

6. Thermal Diffusivity Calculation Calculation First determine the baseline and maximum rise to give the temperature difference, ΔT max Determine the time required from the initiation of the pulse for the rear face temperature to reach ΔT ½. This is the half time, t ½. Calculate the thermal diffusivity, a, from the specimen thickness, L squared and the half time t ½, as follows: Α = 0.13879 L 2 /t ½

7. Determination of Thermal Diffusivity V Time (s) Power source Detector Sample Thermocouple The quantities measured are:temperature (T), time (t) and voltage change (ΔV). Note ΔV ~ ΔT. Experimental Data:

8. Measurement Schematic L Temperature Time Emitted Light Laser Pulse 1us 10.6 um IR Detector Rear Surface Temperature Laser Pulse ΔTmΔTm

9. Real Measurement vs. Adiabatic V t 1/2 1.0 V max 0.5 0 1.0 V t 1/2 1.0 V max 0.5 0 1.0 Adiabatic Real measurement The two graphs show a true measurement vs. an ideal case of no heat loss (i.e. adiabatic): The difference between the two must be accounted for using the correction models contained by the software.

10. Significance and Use Thermal diffusivity is an important property, required for such purposes as design applications under transient heat flow conditions, determination of safe operating temperature, process control, and quality assurance. The flash method is used to measure values of thermal diffusivity, a, of a wide range of solid materials. It is particularly advantageous because of simple specimen geometry, small specimen size requirements, rapidity of measurement and ease of handling, with a single apparatus, of materials having a wide range of thermal diffusivity values over a large temperature range.

11. Thermal Diffusivity It is a measure of how well a material can transmit heat under transient conditions. Since a material does not just transmit heat, but must be warmed by it as well, the thermal diffusivity involves thermal conductivity, specific heat and density. Characteristics: 1.Thermal diffusivity is always a function of temperature and is directional for anisotropic materials 1.Thermal diffusivity may increase or decrease as a function of temperature, e.g. - graphite and many ceramics decrease with temperature - many metal alloys increase with temperature 3.Thermal diffusivity maybe dominated by the electronic or lattice contributions depending upon the type of material

12. The System II

13. The Instrument Detector Furnace Laser / Xenon pulse source

14. The Specifications Modular Design Different furnaces-125 up to 500°C RT up to 500°X RT up to 1250°C RT up to 1600°C Different pulse sourceXenon or Laser pulse source (exchangeable) Different SensorsMCT detector (cryogenic application) InSb detector (standard) Sample robotround samples up to 6 samples 10 mm diameter up to 6 samples 12,7 mm diameter up to 3 samples 25,4 mm diameter square samples up to 6 samples 10x10 mm liquid samples Aluminum / Sapphire / Platinum

15. XFA 500 Xenon Flash Detector Iris Furnace Sample Carrier Xenon Flash

16. LFA 1000 Laser Flash Detector Iris Furnace Sample Carrier Laser

17. Technical Specifications

18. Sample Holders

19. Sample Holders II

20. Sample Holder For Liquids Sample container Crucible Sample container Lid Liquid

21. Sample Preparation Samples are normally coated with a graphite film before testing. The graphite serves several purposes. When testing samples that do not naturally have a high value of emissivity or absorptivity, the graphite increases the energy absorbed on the laser side (bottom) and increases the temperature signal on the detector side (top) of the sample. Also, a uniform graphite coating applied to both sample and reference material helps maintain similar absorptive and emissive efficiencies among samples, which is needed for accurate specific heat measurements. Sample Graphite coating

22. Application Areas 0.00110000.011001100.1 Thermal Conductivity (W/m-K) GASES LIQUIDS INSULATION SYSTEMS NONMETALLIC SOLIDS PURE METALS ALLOYS Hydrogen Oils Carbon dioxide WaterMercury Foams Vacuum Isolation Fibers IcePlastics Aluminum Oxides Nickel SilverZinc

23. Application Areas II Silver, Copper, Silicon Carbide 0.00110000.0101001.0010.00.100 Thermal Conductivity (W/m-K) Vacuum Isolation Air, Polystyrene, PUR Foams Fiber boards, Fiber Insulation Building boards, Oils Wood, Polymers, CoalWater Concrete, Glass, Fiber clay Porous Ceramics, Refractories Alumina SilicatesSilicon nitrideAlumina, Carbon Bricks Iron, Steel SiliconAluminum, Graphite Diamond Flash (-125 …2400°C) Hot Wire (RT…1500°C) Guarded Heat Flow Meter (-150…300°C) Guarded Hot Plate (-180…650°C) Heat Flow Meter (-20…100°C)

24. The Software Software All thermo analytical devices of LINSEIS are PC controlled, the individual software modules exclusively run under Microsoft ® Windows® operating systems. The complete software consists of 3 modules: temperature control, data acquisition and data evaluation. The Linseis 32 – bit software encounters all essential features for measurement preparation, execution and evaluation, just like with other thermo analytical experiments. Due to our specialists and application experts LINSEIS was able to develop this easy understandable and highly practical software.

25. Applications

26. TC vs. Sample Thickness Thermal Diffusivity (cm 2 /s) High Purity Copper (398 W/m*K) Graphite (88 W/m*K) 1.5 Sample Thickness (mm) 1.0 0.5 0.0 Iron (76.8 W/m*K) 0.110

27. TC vs. Temperature

28. PTFE

29. PTFE Applications Chemical processing and petrochemical sectors: used for vessel linings, seals, spacers, gaskets, well-drilling parts and washers, since PTFE is chemically inert and resistant to corrosion Laboratory applications: Tubing, piping, containers and vessels due to resistance to chemicals and the absence of contaminants attaching to the surface of PTFE products Electrical industry: used as an insulator in the form of spacers, tubing and the like Virgin PTFE had been approved by the FDA for use in the pharmaceutical, beverage, food and cosmetics industries in the form of conveyor components, slides, guide rails, along with other parts used in ovens and other heated systems. Semiconductor sector: used as an insulator in the production of discrete components such as capacitors and in the chip manufacturing process.

30. Thermal Diffusivity

31. Combined Result

32. Ceramics

33. Thermal Diffusivity

34. Combined Results

35. Inconel 600

36. Thermal Diffusivity

37. Thermal Conductivity

38. Application Example: Graphite (Polycrystalline) Graphite is an excellent material for checking the performance of a Laser/Xenon Flash Thermal Analyzer. The analyzed material shows a maximum thermal diffusivity around room temperature. The specific heat of the material which can be analyzed by comparative method or by using a DSC / High Temperature DSC shows a significant increase at higher temperatures.

39. Application Graphite

40. Application Example: Aluminum & Copper The pure metals Copper and Aluminum are used in this example to demonstrate the performance of the Linseis Laser Flash device. The measurement results of the two materials are compared with literature values. The measured results vary within 2% of the given literature values; this demonstrates the excellent performance of the instrument.

41. Application: Aluminum & Copper

42. Application Example: Isotropic Graphite (AIST) This graph shows the Thermal Diffusivity values measured on a Linseis LFA 1000 compared to the values measured at AIST* Japan. The literature values of the used Isotropic Graphite from AIST* the measured results on the LFA 1000 vary by less than 2%. *(National Institute of Advanced Industrial Science and Technology, Japan)

43. Isotropic Graphite (AIST)

44. The Best Method Best method for measuring Thermal Diffusivity →Thermal Conductivity The flash method is the most accurate and fastest way of measuring the thermal diffusivity. It has bee estimated that world-wide over 80% of the thermal diffusivity measurements are conducted using the laser flash system

45. Advantages of Flash Diffusivity Measurement 1.Easy sample preparation because of simple geometry Sample sizes are typically 12,7 or 25,4 mm Ø or 10mm square and range from 0.1 to 6 mm thick. 2.Less material is required because of small samples: Some test methods used to measure thermal conductivity directly require very large samples i.e. 30cm x30cm x 5cm in some case 3.Fast measurement time due to small samples: With small samples steady state is reached quickly. Some thermal conductivity methods require days to complete a set of measurement. 4.High accuracy: Depending upon the material accuracies of +/- 3-4% or better can be usually achieved 5.Wide thermal diffusivity / thermal conductivity range: Thermal diffusivity:0.001 to 10 cm 2 /s Thermal conductivity:0.01 to 2000 W/m-K