THERMAL ANALYSIS & THERMO-PHYSICAL PROPERTIES

Transcription

1 THERMAL ANALYSIS & THERMO-PHYSICAL PROPERTIES

2 Introduction 3 DSC Differential Scanning Calorimeter 4 STA Simultaneous Thermal Analysis 6 HDSC / DTA High Temperature DSC/DTA 12 DIL Dilatometry 14 TMA Thermomechanical Analysis 18 EGA Gas Analysis/Couplings 20 LFA/XFA Thermal Diffusivity/Thermal Conductivity 22 HFM 24 THB Transient Hot Bridge 25 LSR-Seebeck 26 Software 27

3 Claus Linseis Managing Director Since 1957 LINSEIS Corporation has been delivering outstanding service, know how and leading innovative products in the field of thermal analysis and thermalphysical properties. We are driven by innovation and customer satisfaction. Customer orientation, innovation, flexibility and high quality are what LINSEIS strives for.thanks to these fundamentals our company enjoys an exceptional reputation among the leading scientific and industrial companies. LINSEIS has been offering benchmark products in highly innovative branches for many years. in sectors such as polymers, chemical industry, inorganic building materials as well as environmental analytics. In addition, Thermophysical properties of solids, liquids and smelts can be analyzed. LINSEIS Corp.thrives for technological leadership. We develop and manufacture thermo analytic and Thermophysical testing equipment to the highest standard and precision. Do to our innovative drive and ultimate precision, we are a leading manufacturer of Thermal Analysis equipment. The development of thermo analytical testing machines requires significant research and a high degree of precision. LINSEIS Corp. invests in this research to the benefit of our customers. The LINSEIS business unit of thermal analysis is involved in the complete range of thermo analytical equipment for R&D and quality control 3

4 DSC Differential Scanning Calorimeter Differential Scanning Calorimetry (DSC) is the most popular thermal analysis technique. It measures endothermic and exothermic transitions as a function of temperature - Endothermic = heat flows into a sample - Exothermic = heat flows out of the sample The instrument is used to characterize polymers, pharmaceuticals, foods/biologicals, organic chemicals and inorganics. Transitions measured include Tg, melting, crystallization, curing and cure kinetics, onset of oxidation and heat capacity.

5 DSC PT 10 DSC PT 10 The Temperature modulated DSC PT10 comprises the advantages of latest technology, highest resolution and a robust easy to use instrument design. The measurement principle of heat flux allows ultimate measurement precision. The sensor has a very high resolution and can be calibrated very accurately. The optional software controlled gas box enables Oxidation Induction Time (OIT) measurements. The Kinetic software and many other features provide the perfect solution for any calorimetric experiment. Food The three evaluated substances (Fructose,Glucose and Saccharose) show distinctive melting points. These melting points can be precisely determined by means of Differential Scanning Calorimetry (DSC). For this the analytical method is frequently used for the determination of unknown substances. Even mixtures with identical molecular weight such as Fructose and Glucose can thus be recognized. DSC PT 10 Thermoplasts PolyEthylenTherephtalat (PET) shows a significant endothermic glass point at about 77 C, which is quite special for partly crystalline thermoplasts. The relation between the exothermal cold crystallization at 131 C and the endothermic melting peak is a measure for the degree of crystallization of the material. In the case of (PET) the crystalline part is very small which results in a good transparency of the material. Friedman analysis lg (dx/dt / [1/s]) /T [1000/K] Friedman analysis with baseline optimization DSC PT 10 Temperature Range -150 up to 700 C Heating and cooling rates Temperature modulation Resolution Cooling Gas control box Atmosphere 0.01 up to 100 C/min available 0.125µW air, LN 2, intracooler up to 4 gases inert, oxid., red. 5

6 STA Simultaneous Thermal Analysis Simultaneous TGA-DTA/DSC measures both heat flow and weight changes in a material as a function of temperature or time in a controlled atmosphere. Simultaneous measurement of these two material properties not only improves productivity but also simplifies interpretation of the results. The complimentary information obtained allows differentiation between endothermic and exothermic events which have no associated weight loss (e.g., melting and crystallization) and those which involve a weight loss (e.g., degradation).

7 STA PT1000 STA PT1000 The LINSEIS STA PT1000 is a top loading Thermobalance, which offers a highly user-friendly design. Even at a sample weight of up to 10g the Tare is done electronically. The specially designed furnaces allow fast heating and cooling rates as well as a highly precise temperature control. Exchanging the different TGA, DTA or DSC measuring systems is only a question of minutes. The STA PT 1000 and STA PT1000 HiRes combine both, the sensitivity of a Thermobalance and true Differential Scanning Calorimeter. Several different TG, TG-DTA and TG-DSC sample holders can be used to determine different reaction- and transition temperatures, enthalpies and specific heat. Thus the system can be perfectly adjusted for any type of application. STA PT 1000 Because of the vacuum tight design of the instrument, static and dynamic atmospheres are possible. In addition a gas control box and a vacuum pump can be connected optionally. Applications Oxidative/Thermal Stability of Materials Composition of Multi-component Systems Estimated Lifetime of Products Decomposition Kinetics of Materials The Effect of Reactive Atmospheres on Materials Moisture and Volatiles Content of Materials Transition Temperatures Heats of Fusion and Reactions Melting and Boiling Points Features Highest precision TG/DTA/DSC Highest resolution Drift stability Exchangeable measuring systems TG-DTA/DSC Different sensor Types E/K/S/B for highest precision measurements at any temperature Evolved gas analysis (MS/FTIR) possible True DSC sensor for Enthalpy & Specific Heat User friendly Software STA PT 1000 STA PT 1000 Hi Res Temperature range RT up to 1000 C RT up to 1000 C Sample Mass 10 g 5 g Resolution 0.5 µg 0.1 µg Measuring system E/K/S E/K/S Vacuum 10 E -2 mbar 10 E -2 mbar TG DTA/DSC Pressure E/K/S Sample carriers DSC measuring system TG DTA/DSC E/K/S 7

8 STA PT 1600 STA PT 1600 The STA PT1600 is the high end Simultaneous Thermobalance from LINSEIS. The system offers unparalleled TG and DSC resolution in combination with highest vacuum capabilities and TG drift stability. The system is modular due to five exchangeable furnaces, many different measuring systems and crucibles. The coupling ability and many other optional accessories guarantee the perfect setup for whatever application. The STA PT 1600 and STA PT1600 HiRes combine both, the sensitivity of a Thermobalance and true Differential Scanning Calorimeter. Several different TG, TG-DTA and TG-DSC sample holders can be used to determine different reaction and transition temperatures, enthalpies and specific heat. Thus the system can be perfectly adjusted for any type of application. Because of the vacuum tight design of the instrument, static and dynamic atmospheres are possible. In addition a gas control box and a vacuum pump can be connected optionally. The evolving gases can be analyzed with our integrated QMS, FTIR or In-Situ EGA coupling options. Sample Robot STA PT 1600 Simultaneous TG-DSC optional Pressure STA PT 1600 Temperature range -150 up to 500 C RT up to 1400/1600/1750 C STA PT 1600 Hi Res -150 up to 700 C RT up to 1500 C/1650 C RT up to 2000/2400 C Sample Mass 25 g 5 g Resolution 0.5 µg 0.1 µg Measuring system E/K/S/B E/K/S/B Atmosphere Inert, oxid., red., vac. Inert, oxid., red., vac. Vacuum 10 E -5 mbar 10 E -5 Pressure optional 2/5 bar Sample carriers TG DTA/DSC TG DTA/DSC DSC measuring system E/K/S/B E/K/S/B 8

9 TG/STA L81-I TG/STA L81-I The LINSEIS L81 is designed as a top loading Thermobalance, providing excellent drift stability, a robust design and highest TG and DSC/ DTA reproducibility. All measuring systems are easily user exchangeable to ensure quick and simple system handling. The broad selection of furnaces (optional turntable) ranging from 150 C up to 2400 C and the large sample mass of up to 25g/3ml are unique features of this system. The balance design provide for high vacuum (10E-5mbar), inert, reducing, flowing or humidified atmosphere. Corrosive conditions can be analyzed with proper precautions. The system is capable of adapting residual gas analysis systems using an optional heated capillary. Because of the vacuum tight design of the instrument, static and dynamic atmospheres are possible. An optional gas control box and a vacuum pump can be connected. up to 2400 C Simultaneous TG-DSC TG/STA L81-I Horizontal/Vertical TG/STA L 81 Temperature Range -150 up to 500 C RT up to 1600 C RT up to 1750 C RT up to 2000 C RT up to 2400 C Sample mass 25g Resolution 1 µg Measuring system Vacuum Automatic evacuation Gas control (optional) Sample holders E/K/S/B 10 E -5 mbar optional up to 4 gases TG / TG-DSC / TG-DTA 9

10 High Pressure STA High Pressure STA Thermogravimetry is a technique in which the mass of the sample is monitored against time or temperature while the temperature of the sample, in a specified atmosphere, is programmed. This technique serves the determination of material compositions. Simultaneous TGA-DTA/DSC measures both heat flow (DSC) and weight changes (TGA) in a material as a function of temperature or time in a controlled atmosphere. Simultaneous measurement of these two material properties not only improves productivity but also simplifies interpretation of the results. The complementary information obtained allows differentiation between endothermic and exothermic events which have no associated weight loss (e.g., melting and crystallization) and those which involve a weight loss (e.g., degradation). The High Pressure LINSEIS STA (simultaneous thermal analysis) delivers unsurpassed performance. The system can be used to determine simultaneous changes of mass (TG) and caloric reactions (HDSC) under defined atmosphere and pressure (up to 150 bar) in the temperature range RT C. This instrument is worldwide the only available pressure STA. The unique characteristics of this product are high precision, high resolution and long term drift stability. The STA Platinum Series was especially developed to meet the challenging demands of the high temperature as well as high pressure applications. up to 150 bar HP STA up to 1800 C STA HP/1 STA HP/2 Temperature range RT up to 1000 C -170 up to 1400/1600/1800 C Heating element Kanthal SiC or Graphite Pressure range up to 150 bar up to 50 bar Vacuum up to 10 E -4 mbar up to 10 E -4 mbar TG resolution 0.1/0.5/10 µg 0.1/0.5 µg Sample weight 2/15/100 g 2/15 g TG-DTA/DSC measuring systems E/K/S/C E/K/S/B/C Atmosphere inert, oxid., red., vac. inert, oxid.*, red., vac. *not possible with graphite heater 10

11 Magnetic Suspension Balance - MSB Magnetic Suspension Balance - MSB With the magnetic suspension balance gravimetric measurements in a wide temperature and pressure range and under aggressive media can be done. Such a magnetic suspension balance consists of a balance for recording the measurement values, a suspension coupling which carries the weight of the sample, a sensor for the position measurement of the levitation part and a control unit to control the suspension coupling. The contact-less transmission of the sample weight is realized with a levitation magnet and a holding magnet. The levitation magnet consists of a permanent magnet and the holding magnet consists of an electromagnet hanging on the balance. The position sensor delivers the actual position of the levitation magnet and the PID controller makes a stable levitation position with the electromagnetic force as the actuating variable. Through the magnetic coupling a micro balance can be set up at environmental condition. Therefore the balance is protected from high temperatures, pressure and aggressive media. MSB PT 1 Magnetic Suspension Corrosive Atmospheres up to 150 bar Metal Version Glass Version Pressure range UHV to 150 bar Vacuum to 1.3 bar Temperature range -196 to 2400 C up to 900 C Sample weight 10 g (standard balance) 10 g (standard balance) Resolution 1 µg 1 µg Evolved Gas Analysis MS/FTIR possible MS/FTIR possible Special custom versions can be realized! 11

12 HDSC / DTA High Temperature DSC/DTA Differential Scanning Calorimetry (DSC) is the most popular thermal analysis technique it measures endothermic and exothermic transitions as a function of temperature - Endothermic = heat flows into a sample - Exothermic = heat flows out of the sample Linseis offers a unique line of high temperature DTA and DSC systems.

13 High Temperature DSC High Temperature DTA High Temperature DSC/DTA PT1600 This is the most common thermal analysis method due to its wide range of information provided. The LINSEIS high temperature DTA/DSC is designed to deliver highest calorimetric sensitivity, short time constants and a condensation free sample chamber. These features guarantee superior resolution, baseline stability over the entire instrument lifetime. Thus providing a indispensable tool for material development, R&D and quality control. The modular concept of the DSC and DTA systems allows the use of different furnaces with a temperature range from -150 up to 2400 C, different measuring systems for DSC and DTA as well as many different crucibles. The vacuum tight design enables quantitative enthalpy and Cp (Specific Heat) determination under cleanest atmospheres as well as under vacuum 10E-5mbar. Additionally the systems can be coupled to a MS or FTIR. DSC/DTA PT 1600 DSC Sample Robot DTA DSC-Cp DTA, DSC, DSC Cp Highest Resolution DSC PT 1600 DTA PT 1600 Temperature range -150 up to 500 C RT up to 1400 C RT up to 1500 C RT up to 1600 C RT up to 1650 C RT up to 1750 C -150 up to 500 C RT up to 1400 C RT up to 1500 C RT up to 1600 C RT up to 1650 C RT up to 1750 C RT up to 2000 C RT up to 2400 C Sensors E/K/S/B DSC-C P, DSC, DTA different sensors Vacuum 10-5 mbar 10-5 mbar Atmospheres inert, oxid., red., vac. inert, oxid., red., vac. Temperature modulation yes yes 13

14 DIL Dilatometry Dilatometry (DIL) is a technique in which a dimension of a substance under negligible load is measured as a function of temperature while the substance is subjected to a controlled temperature program in a specified atmosphere. Dil L75 Vertikal

15 DIL L 76 PT DIL L75PT Horizontal / Vertical DIL L 76 PT The LINSEIS Dilatometer series L76 PT combines user friendliness and high modularity to different applications with outstanding performance in one system. The low cost dilatometer series is especially suitable for the ceramics and glass industry. DIL L76 DIL L75PT Horizontal / Vertical The high end pushrod dilatometer solves all measurement tasks when it comes to determining the thermal length change of solids, powders or pastes. The horizontal / vertical design as single or differential system provides the perfect solution for any type of expansion coefficient and material characteristics. All models rely on a LVDT displacement sensor with almost indefinite resolution, furthermore the thermostatically controlled housing and perfect measuring design allow the highest precision and resolution measurements as well as long term drift stability. DIL L75 1, 2, 4, 8 Samples -180 to 2800 C up to 3 Furnaces DIL L 76 PT DIL L 75 PT Horizontal DIL L 75 PT Vertical Temperature range RT up to 1000/1400/1600 C -180 up to 500 C RT up to 1000/1400/1600/2000 C -180 up to 500 C RT up to 1000/1400/1600/ 17500/2000/2400/2800 C Resolution 1.25 nm/digit nm/digit nm/digit Sample lenght 25/50 mm 25/50 mm 25/50 mm Sample diameter 7/14/20 mm 7/14/20 mm 7/14/20 mm Sample number single or differential single or differential single, differential or quattro Atmosphere inert, oxid. inert, oxid., red., vac. inert, oxid., red., vac. Sample holders fused silicia, Al 2 O 3, sapphier fused silicia, Al 2 O 3, sapphier, graphite fused silicia, Al 2 O 3, sapphier, graphite 15

16 L 75 Laser Dilatometer DIL L 74 Optical Dilatometer Laser Dilatometer The Laser Dilatometer is the next step in expansion measurements. The L75 Laser Dilatometer outperforms any conventional pushrod dilatometer by offering a 33 times higher resolution. The measurement principle is based on a Michelson interferometer thus eliminating all mechanical errors. Pico Resolution Applications Highest precision expansion measurements of materials such as: Carbon, Graphite, Composite materials, Glass, Alumina, Fused Silica, Substrates, semiconductor material, etc Quality and entry control of materials with problematic expansion characteristics like, glass, bimetals, precision electronics components, etc. L 78 RITA L75 Laser Dilatometer Method Laser Dilatometer Michelson Prinzip Temperature Range -180 up to 500 C; RT up to 1000 C Sample dimensions Resolution Atmosphere Vacuum up to 20 mm long and up to 7 mm diameter 0.3 nm inert, oxid., red., vac. 10 E -5 mbar DIL L 74 Optical Dilatometer The Optical Research Dilatometer L74 was developed to meet the demanding applications of the glass, ceramics, metal and energy industry. A high resolution CCD camera enables a visual real time analysis of the sample expansion, either as single frame or as video sequences. Several correction and analysis features are incorporated into the LINSEIS Evaluation Software. The unique horizontal design enables most demanding applications. The special solid-liquid adapter allows expansion / volume measurements of solids, liquids and solid liquid phase transitions. DIL L74 Applications Heating microscope Optical Fleximeter Non contact Expansion measurement Sessile Drop Contact angle Solid-liquid expansion (optional adapter) Non Contact DIL L 74 Temperature range C, RT up to 500/ 1000/1400/1600 C Measuring system optical non contact Accuracy up to 1μm Atmosphere oxidizing, (optional: reducing, inert, and vacuum) 16

17 Quenching /Deformation Dilatometer Quenching /Deformation Dilatometer The Quenching Dilatometer L78 RITA is especially suitable for the determination of TTT, CHT and CCT diagrams. The special induction furnace enables heating and cooling speeds in excess of 400 C/s. The system complies with ASTM A1033. All critical parameters such as heat up and cool down speed, gas control and safety features are software controlled. The professional 32-bit software Linseis TA-WIN operates exclusively under the Microsoft operation system. All routine (creation of CHT/CCT/TTT diagrams) and demanding applications are solved by the unique Software package which comes with the instrument. Certainly export functions in ASCII-format as well as graphic output is possible. up to 2500 C/s Picture Dr. Sommer Werkstofftechnik GmbH, Issum TTT, CHT, CCT L 78 RITA/Q Quenching Dilatometer L 78 RITA/Q/D Deformation Dilatometer Temperature Range -100 up to 1600 C -100 up to 1600 C Sample geometry solid and hollow samples solid samples Sample diameter approx. 4 mm approx. 5 mm Sample length approx. 10 mm approx. 10 mm Heating/cooling rates 2500 C/s 400 C/s Defromation force Deformation rate Minimum pause between two 25 kn ( mm)/s 60 ms deformation steps 17

18 TMA Thermomechanical Analysis Thermomechanical analysis (TMA) measures linear or volumetric changes in the dimensions of a sample as a function of time, temperature and force in a controlled atmosphere.

19 TMA PT1000 TMA PT1000 The Thermomechanical Analyzers TMA PT1000 and TMA PT1000 EM uniquely combine the flexibility of several measurement procedures under changing requirements. The instrument can measure expansion and deformation at highest precision. TMA PT 1000 TMA PT 1000 EM TMA PT 1000 Temperature Range -150 up to 1000 C -150 up to 1000 C Cryo option available available Force 1/5.7 N 1/5.7/20 N Frequency 1/5 Hz Resolution nm nm Atmosphere inert, oxid., red., vac. inert, oxid., red., vac. Vacuum 10 E -5 mbar 10 E -5 mbar TMA PT1600 The TMA PT1600 offers a broad temperature range (RT up to 1600 C) for all kinds of Thermomechanical investigations. The system can perform either static or dynamic experimentes. Typical materials under investigation are: composites glass ceramics metals polymers TMA PT 1600 TMA PT 1600 Temperature Range -150 up to 500 C RT up to 1600 C Force Frequency Resolution Atmosphere Vacuum 1 N 1 Hz nm inert, oxid., red., vac. 10 E -5 mbar 19

20 EGA Gas Analysis/Couplings When coupling a Thermal Analyzer with a Quadrupole Massspectrometer (QMS) or FTIR (Fourier Transformed Infrared Spectrometer) out gassing products can be determined and identified. The signal can then be time wise correlated with the signals received by the Thermal Analyzer. With the optional Pulse Analysis the outgasings can be quantified when using a QMS as well as a FTIR.

21 Evolved Gas Analysis In-Situ EGA Evolved Gas Analysis The combination of a LINSEIS Thermal Analyzer with a FTIR (Fourier Transformed Infrared Spectrometer) is especially interesting in fields such as polymers, chemical and pharmaceutical industry. The coupling is more than the sum of the separate parts. Benefit from LINSEIS coupling knowledge and integrated hard- and software concept MS coupling Mass numbers Detector Vacuum system Heating Couplings 100/200/300 amu Faraday and SEV (Channeltron) Turbomolecular and Diaphragm pump (oil free) adapter, heated capillary and QMS DSC, TGA, STA, DIL by heated cappilary FTIR coupling Wave numbers cm -1 Resolution 1 cm -1 Heating Transfer line and adapter: up to 230 C Material transfer line PTFE (exchangeable) In-Situ EGA Main advantages Direct detection of gas compounds, not only mass numbers Real time in-situ measurement method No intrusion into the measurement system (as for extracting systems) No cooling of the analyzed gas No condensation of substances with high condensation temperatures No equilibrium shifts because of temperature changes No contamination of the sample gas in extracting lines Allows usage of principally all optical gas measurement systems (tested for FTIR, Raman, ELIF, among others) Raman-Spectroscopy Measurement of basic gas components Also not polar molecules like H 2 or N 2 are measurable ELIF: Excimer Laser induced Fragmentation Fluorescence UV-Laser-based Method for measuring of gaseous alkaline compounds (for example NaCl, NaOH, KCl, KOH). Also at 193 nm a entry through UV-Sapphire is possible Overview of proven Measuring Methods FTIR: Fourier Transform Infrared Spectroscopy Measurement of basic and trace gas components until ppm range, for example H 2 O, CO 2, CO, H 2 S,.. Polar Molecules are necessary 21

22 LFA/XFA Thermal Diffusivity/ Thermal Conductivity The sample is positioned horizontally on a sample robot, located in a furnace. The furnace is then held at a predetermined temperature. At this temperature the sample bottom is then irradiated with a programmed energy pulse (laser or xenon flash). This energy pulse results in a homogeneous temperature rise at the sample top. The resulting temperature rise of the sample top is measured by a high speed IR detector and thermal diffusivity values are computed from the temperature rise versus time data. The resulting measuring signal computes the thermal diffusivity, and in most cases the specific heat (Cp) data. If the density (r) is identified, the thermal conductivity can be calculated: l(t)=a(t) Cp(T) r(t)

23 Laser Flash/Xenon Flash Laser Flash/Xenon Flash LINSEIS offers a variety of instruments to measure the Thermal Diffusivity. The XFA 500 provides a cost effective solution for the temperature range RT up to 500 C. The highly modular design allows upgrade to the LFA 1000 the high end system whenever the measurement requires or the budget allows it. The LFA 1000 provides unbeaten sampling rates, up to 6 samples at the same measurement cycle, highest modularity, three different user exchangeable furnaces (-125 up to 1600 C) and two detectors as well as a high vacuum design (10E-5 mbar). System Design LINSEIS is offering an unparalleled modular system design for this Thermophysical properties Analyzer. It is possible to upgrade the temperature range (exchangeable furnaces/ measuring system) and the detector (InSb/MCT). This enables the user to start with a cost effective solution and upgrade the system whenever the budget allows or the measurement task requires it. Correspondence with International Standards. The LINSEIS LFA and XFA operate in agreement with national and international standards such as ASTM E-1461, DIN and DIN EN 821. Thermal Conductivity l XFA 500/LFA 1000 Multiple Furnaces Sample Robot XFA 500 LFA 1000 Sample dimension ø 6 to 25.4 mm diameter; 0.1 to 6.0 mm height ø 6 to 25.4 mm diameter; 0.1 to 6.0 mm height Maximum sample number up to 6 samples up to 6 samples Temperature range RT up to 500 C -125 up to 500 C RT up to 1250 C/1600 C Vacuum 10 E -5 mbar 10 E -5 mbar Atmoshere inert, oxid., red., vac. inert, oxid., red., vac. Thermal Diffusivity 0.01 up to 1000 mm 2 /s 0.01 up to 1000 mm 2 /s Thermal Conductivity 0.1 up to 2000 W/(m K) 0.1 up to 2000 W/(m K) Pulse source Xenon Flash Nd: YAG Laser Pulse enery 10 J/Puls 25 J/Puls 23

24 HFM 300 / 600 LINSEIS HFM 300 / 600 This Heat Flow Meter provides a rapid and easy to use instrument to determine the thermal conductivity properties of low thermal conductivity insulation materials and other materials with a high level of accuracy. The instrument is designed per ASTM C518, JIS A1412, ISO 8301 and DIN The principle of measurement is to position a sample between a hot and a cold plate, and to measure the heat flow. Service and Maintenance The robust system design and the unique zero maintenance Peltier heating and cooling cycle ensure a minimum of upholding cost. Test Cycles The double heat flux sensor configuration ensures shortest possible measurement cycles. A typical measurement for most samples can take as little as 15 minutes until the temperature stabilizes. HFM 300/600 Sample Thickness Two heat flux sensor then measures the heat flow which is precisely defined between the hot and cold plate. Building Industry Direction of heat flow LVDT System Heat source (Heating foil) Peltier system Hot plate Heat flux transducer Test sample Heat flux transducer Cold plate W/m K Heat sink (Peltier system) HFM 300/1 HFM 300/2 HFM 300/3 HFM 600/1 Temperature range (Plates) Fixed, 0 to 40 C Variable, 0 to 100 C Variable, -30 to 90 C Variable, -20 to 70 C Cooling system Forced Air Forced Air External Chiller External Chiller Temperature control (Plate) Measurement Data Points Peltier Peltier Peltier Peltier Sample size 300x300x100 mm 3 300x300x100 mm 3 300x300x100 mm 3 600x600x200 mm 3 Thermal resistance measuring range Thermal Conductivi ty Measuring Range 0.1 to 8.0 m 2 K/W 0.1 to 8.0 m 2 K/W 0.1 to 8.0 m 2 K/W 0.1 to 8.0 m 2 K/W to 0.5 W/m K to 0.5 W/m K to 0.5 W/m K to 0.5 W/m K Reproducibility 0.5% 0.5% 0.5% 0.5% Accuracy +/- 1 to 3% +/- 1 to 3% +/- 1 to 3% +/- 1 to 3% 24

25 THB Transient Hot Bridge THB Transient Hot Bridge The Transient Hot Bridge technique enables thermal conductivity, thermal diffusivity and specific heat measurements on various sample geometries and materials. This LINSEIS measuring instrument provides the three material properties simultaneously after just a few minutes time regardless of whether you have used the patented sensor in a solid matter (incl. bulk material, gels, pastes) or in a liquid. The preparation of solid samples is pretty simple: One plane surface of two sample halves is sufficient for the sensor. Reference or calibration measurements are a thing of the past. As a matter of course, the THB measures absolute values, with an uncertainty which is not behind that of conventional plate or our laser flash devices. Different sensors, easily exchanged, are available for laboratory and field use. The THB measures fully automatically. Its software control optimizes the measurement process independently, aiming at a short duration and a minimum uncertainty. In addition, it continuously monitors a possible temperature drift of the sample. Due to the short measurement times, serial measurements can be performed at a forced sequence and with a high sample output. In addition to the measurement values, the Software calculates and displays the associated measurement uncertainties in accordance with the international ISO standard. Thermal Conductivity l Result in 1 Minute Fully automatic Measuring ranges Thermal Conductivity 0.01 to 50 W/(m K) Thermal Diffusuvity 0.05 to 10 mm 2 /s Special thermal capacity 100 to 5000 kj/(m 3 K) Measurement uncertainties Thermal Conductivity better than 2% Thermal Diffusuvity better than 5% Special thermal capacity better than 5% Duration of the measurement minutes Service temperature Sensor -100 to 200 C or -100 to 600 C Sensor type Kapton and Ceramic insulated sensor Sample size Smallest sample Sample consistency 3 x 3 x 3 mm solid, liquid, gel, powder, granulate 25

26 LSR-3 Seebeck LSR-3 Seebeck The Thermal power, thermoelectric power, or Seebeck coefficient of a material measures the magnitude of an induced thermoelectric voltage in response to a temperature difference across that material. The thermal power has units of (V/K). In recent years much interest has been shown in various methods of direct conversion of heat into electricity. Waste heat from hot engines and combustion systems could save billions of dollars if it could be captured and converted into electricity via thermoelectric devices. For this challenging application Linseis has developed a characteristic evaluating instrument for these materials and devices; the LSR -3 LINSEIS - Seebeck & Electric Resistivity Unit. Features The LSR - 3 can simultaneously measure both Seebeck coefficient and electric resistance (Resistivity). Prism and cylindrical samples with a length between 6 to 23mm can be analyzed Wires and Foils can be analyzed with a unique measurement adapter Three different exchangeable furnaces cover the temperature range from -100 up to 1500 C The design of the sample holder guarantees highest measurement reproducibility State of the art 32-Bit software enables automatic measurement procedures Measurement Data can be easily exported the measuring arrangement heats the sample to a specified temperature. At this temperature the secondary heater in the lower electrode block creates a set temperature gradient. Two contacting thermocouples then measure the temperature gradient T1 and T2. A unique thermocouple contact mechanism permits highest temperature accuracy measurements of the electromotive force de at one wire of each of the two thermocouples. The dc four-terminal method is used to measure the Electric Resistance. By applying a constant current (I) at both ends of the sample and measuring the change in voltage dv between one wires at each of the two thermocouple pairs. LSR-3 Seebeck Principles of Measurement A sample of cylindrical or prism shape is vertically positioned between two electrodes. The lower electrode block contains a heater, while the entire measuring arrangement is located in a furnace. The furnace surrounding LSR 3 Temperature Range Measurement method -100 up to 500 C; RT up to 800/1100/1500 C Seebeck coefficient: Static dc method Electric resistance: four-terminal method Specimen holder Atmosphere Sample size Lead interval Cooling water sandwiched between two electrodes inert, oxid., red., vac. 2 to 4 mm 2 or diameter x 6 to 23 mm long 4, 6, 8 mm required 26

27 Software LINSEIS TA-WIN Features -Software: User-friendly Multi-methods analysis (DSC TG, TMA, DIL, etc.) Zoom function Online help menu Report generator Data export to MS Excel Export and import of data ASCII Program capable of text editing Data security in case of power failure Thermocouple break protection Repetition measurements with minimum parameter input Evaluation of current measurement Curve comparison up to 32 curves Storage and export of evaluations Programmable gas control Statistical evaluation package Smoothing of total or partial measurement Tangent intersection determination (automatic or manual) Free scaling The information of a thermo analytical measurement can be increased when using the broad range of specialized Software. Software Options Specific Heat determination (Cp) Rate Controlled Sintering (RCS) Calculated-DTA Quenching Dilatometer Software CHT / CCT / TTT Diagrams Thermo Kinetics Software 27

28 LINSEIS GmbH Vielitzerstr Selb Germany Tel.: (+49) Fax: (+49) LINSEIS Inc. 109 North Gold Drive Robbinsville, NJ USA Tel.: +01 (609) Fax: +01 (609) Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect Services: Service Lab, Calibration Service