Thermal Analysis

THERMOGRAVIMETRIC ANALYSIS

What is TGA?

Measurement of the weight loss of the materials as a function of temperature. weight loss or gain due to decomposition, oxidation, or dehydration. This technique is suited for many solid materials. characterization information to the most commonly used thermal technique, DSC. Use in all phases of research, quality control and production operation.

 Technique can characterize materials that exhibit

 Provides complimentary and supplementary

What TGA can tell you?

 Composition of Multicomponent Systems  Thermal Stability of Materials  Oxidative Stability of Materials  Estimated Lifetime of a Product  Decomposition Kinetics of Materials  The Effect of Reactive or Corrosive Atmospheres on Materials  Moisture and Volatiles Content of Materials

Parts of TGA instrument

TGA PROCEDURE

Latest TGA

TGA scan example:

Ideal Uses


Thermal stability/degradation investigation of organic or inorganic materials, e.g. polymers, composites, glasses, metals, minerals etc. Thermal stability/degradation investigations in inert or oxidative atmospheres, or in vacuum Determination of organic/inorganic content of mixtures Curing kinetics (e.g, adhesives, polymers) Chemical composition measurements (using appropriate reference standards, accurate quantification of sample composition can be determined Phase transition measurement (e.g. glass transition, clustering, crystallinity, melting point) Quantum - size effect investigation for nanomaterials Reaction kinetics with reactive gases (e.g., oxidation, hydrogenation, chlorination, adsorption/desorption) Pyrolysis kinetics (e.g., carbonization, sintering)

   

   

Strengths of TGA
 Any type of solid can be analyzed, with minimal sample preparation (e.g. powders, pellets, chunks, flakes etc)  Minimum sample size ( at least 0.1mg)  Qualitative or quantitative analysis

Limitations of TGA
 Solid (or initially solid) samples only  Data interpretation not always straightforward. Analysis in combination with other techniques is often helpful.  Limitation are possible reactions may arise with the crucible materials or corrosive gases emitted by the sample.

Relevant Industries for TGA

           

Semiconductor Energy Polymers/biomass Pharmaceutical Biomedical Metallurgy Ceramics Chemicals Construction materials Optical Solar Batteries

References:


Dr. Marissa A. Paglicawan s Lecture 5: Thermal properties of polymers Experimental determination of Tg Thermogravimetric analysis http://www.eaglabs.com/techniques/analytical_techniques/t ga_dta.php Characterization of Polymers Using TGA by W.J. Sichina, Marketing Manager http://micro-scan.com/tga.html http://www.nano-c.com/nanoprod.html http://gideonlabs.com/thermal.htm

    

Thermal Analysis

DYNAMIC MECHANICAL ANALYSIS

What is DMA?
 Technique where a small deformation is applied to a sample in a cyclic manner.  This allows the materials response to stress, temperature, frequency and other values to be studied.

DMA versus TMA

 TMA

Applies a constant static force to a material and watches the material change as temperature or time varies. It reports dimensional changes. It gives coefficient of thermal expansion, or CTE
 DMA

Applies an oscillatory force at a set frequency to the sample and reports changes in stiffness and damping. It gives modulus information

Mechanical Testing

Test configurations

DMA PROCEDURE

Latest DMA

1 2 Log E 3 4

Temperature, C

 Data: Large drop in Er

for T > Tg.

Adapted from Fig. 15.7, Callister 6e. (Fig. 15.7 is from A.V. Tobolsky, Properties and Structures of Polymers, John Wiley and Sons, Inc., 1960.)

10 5 E r (10s) in MPa 10 3 10 1 10 -1 10 -3

rigid solid (small relax) transition region

viscous liquid (large relax)

60

10 0 Tg

140

180 T(C)
(amorphous polystyrene)

Selected values from Table 15.2, Callister 6e.

Reference:
 Dr. Marissa A. Paglicawan s Lecture 5: Thermal

properties of polymers Experimental determination of Tg Thermogravimetric analysis

 Experimental Measurement Of Glass Transition

Temperature by Jia Liu(01-21-10)

 Dynamic Mechanical Analysis (DMA) Basics and Beyond

by Dr. Lin Li (April 2000)

 Introduction to Dynamic Mechanical Analysis (DMA)

by PerkinElmer precisely