Thermal Analysis

Behrend has multiple thermal characterization instruments, which include differential scanning calorimeters (DSC), flash-DSCs, thermogravimetric analyzers (TGA), thermomechanical analyzers (TMA), dynamic mechanical analyzers (DMA), and a thermal conductivity tester. Commonly, multiple thermal instruments are utilized in conjunction to fully characterize a polymer material.

 

The DSC instruments include one Mettler Toledo DSC 1 and two Mettler Toledo DSC 3, including one with an auto sampler. A DSC instrument measures the amount of energy a samples absorbs or releases during heating or cooling, relative to a standard (i.e. the differential aspect of DSC). The temperature range of a DSC3 is -150 °C to 700 °C, with a heating rate of 0.02 K/minute to 300 K/minute. The auto sampler can process up to 34 samples at one time.

Mettler Toledo DSC1	Mettler Toledo DSC3 with auto sampler
Mettler Toledo DSC3

 

The flash-DSC are two Mettler Toledo flash-DSC 1s, for use as fast scanning calorimetry (FSC). The advantage of a flash DSC over a regular DSC is the extremely fast heating and cooling rates; for the DSC1, the heat rate is 1 K/s to 40,000 K/s (60 K/minute to 2,400,000 K/minute).

Mettler Toledo Flash DSC 1

Mettler Toledo Flash DSC

 

The TGA instruments are a Mettler Toledo TGA 1 and a Mettler Toledo TGA 2. TGA instruments measure change in weight/mass as a sample is heated, cooled, or held at a constant temperature. The temperature range for the TGA2 is 30 °C to 1100 °C.

Mettler Toledo TGA1

Mettler Toledo TGA2

 

The TMA instrument is a Mettler Toledo TMA/SDTA 2+. A TMA instrument measures the changes in a sample’s dimensions as a function of time, temperature, and force. The SDTA (single differential thermal analysis) aspect allows for simultaneous measurement of thermal effects on the sample, allowing for correct identification of sample transitions. The TMA/SDTA 2+ has a force range of -0.1 N to 1.0 N, a temperature range of -150 °C to 600 °C.

 

The DMA instruments include a Mettler Toledo DMA/SDTA 861 and a TA Instruments Q800 DMA. DMA instruments measure the stiffness and damping properties as a function of time, temperature, and frequency. The Mettler Toledo DMA has a force range of 1 mN to 40 N, a frequency range from 0.001 Hz to 1,000 Hz, and a temperature range of -150 °C to 500 °C. The SDTA (single differential thermal analysis) aspect allows for simultaneous measurement of thermal effects on the sample. Fixtures for the Mettler Toledo DMA include the single/double cantilever, the 3-point bend, the shear sandwich, the tension clamp, and a compression clamp. The TA Instruments DMA has a force range of 1 mN to 18 N, a frequency range of 0.01 Hz to 200 Hz, and a temperature range of -150 °C to 600 °C. Fixtures for the TA Instruments DMA include the single/double cantilever, the 3-point bend, and the compression clamps.

Mettler Toledo DMA/SDTA 861

TA Instruments Q800 DMA

 

The thermal conductivity tester is a CTherm Trident thermal conductivity instrument. Sensors on this instrument include the MTPS (modified transient plane source) and flex TPS (transient plane source). The MTPS sensor is appropriate for samples with a thermal conductivity between 0 W/mK to 500 W/mK and the test time is 0.8 seconds to 3 seconds. The TPS sensor is appropriate for samples ranging from 0.005 W/mK to 2,000 W/mK thermal conductivity and a test time of 10 seconds to 180 seconds.

 

Sample Specifications

Sample geometries and dimensions are dependent on the technique. Specific sample requirements should be discussed with appropriate staff.

 

Advancing Research

Access to thermal characterization instruments advance the research of faculty members and students in the School of Engineering. Examples of Behrend faculty members using these instruments to expand their research capabilities include:

• Drs. Xiaoshi Zhang, Anne Gohn, and Alicyn Rhoades utilized the TGA, DSC, and FSC. The results shown here are fully explained in this journal article: Zhang, X., Alexander, J. D., Seo, J., Gohn, A. M., Behary, M. J., Schaake, R. P., … & Rhoades, A. M. (2023). Crystallization kinetics of glass fiber filled poly (ether ether ketone) with nanogram sample size: Feasibility study for fast scanning calorimetry. Thermochimica Acta, 721, 179442.
  

  TGA comparison of PEEK, 15 wt% and 30 wt% glass-fiber-filled PEEK 450 G, each at a heating rate of 20 K/min. In each scan, the gas was switched from N2 to air at 600 °C.	DSC melting and crystallization curves (exo up) of neat PEEK, PEEK-15GF, and PEEK-30GF using 20 K/min cooling and heating rates.
  DSC isothermal crystallization exotherms of PEEK at indicated temperatures after cooling at 20 K/min from 400 °C.	Isothermal crystallization peak time of PEEK (black), PEEK-15GF (red), and PEEK-30GF (blue). Crystallization peak times collected from FSC exothermic peaks, FSC indirect method, and DSC exothermic peaks are represented by ■, ●, ▼symbols, respectively. Data for the dashed line is from previous work for unfilled PEEK by Seo et al.

•  Drs. Xiaoshi Zhang, Anne Gohn, Gamini Mendis, and Alicyn Rhoades utilized a flash DSC for their work on polyamide 6 polymers. The images are shown here from this journal article: Zhang, X., Gohn, A., Mendis, G., Buzinkai, J. F., Weigand, S. J., & Rhoades, A. M. (2021). Probing three distinct crystal polymorphs of melt-crystallized polyamide 6 by an integrated fast scanning calorimetry chip system. Macromolecules, 54(16), 7512-7528.
  

  (Left) Melting curves after crystallization at indicated temperatures with predefined crystallization times from 0.1 to 300 s. (Right) Variation of the heat of fusion with time. The t0.5 value was extracted with the logistic equation. The same colors are used in melting curves and their corresponding enthalpy of fusion values.

  

 

Interested in using on of the thermal instruments or having Behrend staff run samples on one of these instruments for you? Please complete our contact page.