Thermal
Gravimetric Analysis (TGA) is a simple analytical technique
that measures the weight loss (or weight gain) of a material
as a function of temperature. As materials are heated, they
can loose weight from a simple process such as drying, or from
chemical reactions that liberate gasses. Some materials can
gain weight by reacting with the atmosphere in the testing
environment. Since weight loss and gain are disruptive
processes to the sample material or batch, knowledge of the
magnitude and temperature range of those reactions are
necessary in order to design adequate thermal ramps and holds
during those critical reaction periods.
A.
Characteristics or Properties Measured
Drying, structural water release, structural decomposition,
carbonate decomposition, gas evolution, sulfur oxidation,
fluoride oxidation, and re-hydration.
Examples of
Applications
The test results are a graph of the TGA signal (actual weight
loss or gain converted to percent weight loss) on the Y-axis
plotted versus the sample temperature in ¡ÆC on the X-axis.
Sample graphs of enhanced standard outputs are shown below.
Structural
Clay Analysis |
Advanced
Ceramics-Oxidation Studies |
|
|
TGA
- Principle of Operation
A sample of the test material is placed into a high alumina
cup that is supported on, or suspended from an analytical
balance located outside the furnace chamber. The balance is
zeroed, and the sample cup is heated according to a
predetermined thermal cycle. The balance sends the weight
signal to the computer for storage, along with the sample
temperature and the elapsed time. The TGA curve plots the TGA
signal, converted to percent weight change on the Y-axis
against the reference material temperature on the X-axis.
Orton
manufactures two basic types of TGA instruments. One uses a
standard pan balance in which the sample cup is supported by a
ceramic post sitting on the balance pan (sketch below left),
and the other uses a higher resolution balance that suspends
the sample cup from overhead (sketch below right).
¡¡
B.
Standard TGA Instruments from Orton
Model TG-730 Series |
Model TG-740 Series |
Model TG-720 Series |
Temperature
Ranges
There are three temperature ranges and four types of furnaces
for those ranges:
- Room Temperature to 1,200¡ÆC
Kanthal wire wound heating element
- Room Temperature to 1,600¡ÆC
Platinum alloy wire wound heating element Silicon Carbide
heating element
- Room Temperature to 1,700¡ÆC
Molybdenum Disilicide heating elements
Type
of Balance
There are four balances used in standard Orton systems. These
balances have been selected based upon the combination of
sample size and weight loss/gain that are typical for most
ceramic material requirements.
Model
Number Series |
TG-
730
|
TG-740
|
TG-720-1000
|
TG-720-2000a
|
TG-720-2000b
|
Sample
Volume (cubic millimeters) |
150
|
150
|
150
|
150
|
150
|
Sample
Size (grams)* |
0.350
|
0.350
|
0.350
|
0.350
|
0.350
|
Range
of % Weight Change |
5
to 33%
|
2
to 20%
|
0
to 100%
|
0
to 100%
|
0
to 100%
|
Max.
Weight Change (grams) |
0.116
|
0.070
|
0.350
|
0.350
|
0.350
|
Min.
Weight Change (grams) |
0.018
|
0.007
|
0.000
|
0.000
|
0.000
|
Balance
Capacity (grams) |
61
|
42
|
100
|
3.500
|
3.500
|
Max.
Balance Change Capacity (grams) |
|
|
10
|
0.150
|
0.750
|
Balance
Sensitivity (grams) |
0.0001000
|
0.0000100
|
0.0000010
|
0.0000001
|
0.0000001
|
Balance
Sensitivity (micro-grams) |
100.0
|
10.0
|
1.0
|
0.1
|
0.1
|
%
Sensitivy of Min. Sample Weight Change |
0.5714%
|
0.1429%
|
0.0000%
|
0.0000%
|
0.0000%
|
%
Sensitivy of Max. Sample Weight Change |
0.0866%
|
0.0143%
|
0.0003%
|
0.0000%
|
0.0000%
|
*
Note: assume a material with a green specific gravity of 2.35
g/cc
Orton has a large
sample option for the TG-730 and TG 740 series balances.
Instead of the 150 cubic millimeter sample cup, a 770 cubic
millimeter cup is available. Other balances and TGA systems
are available for TGA applications requiring even larger
sample sizes, or special samples.
Heating
Rates
Most ceramic samples are normally heated from ambient to the
maximum temperature at 3¡ÆC per minute. Slow heating rates are
preferred so that the weight change can occur over a narrower
time span and temperature range. The resulting curve is
steeper and the onset temperature is closer to the actual.
Fast heating rates spread the weight change over a wider time
span and temperature range, and generate less steep curves and
shift the onset temperature above the actual. Orton control
systems provide the ability to set various heat up rates
according to the user's requirements.
Computer Analysis
All Orton TGA's are supplied with data acquisition and
analysis software for the user's PC. The software displays the
test progress on the monitor, stores the data and enables the
user to perform analysis on the data.
Thermal
Cycle
Most TGA tests are performed at a standard heating rate to the
maximum temperature, then discontinued. The thermal cycle can
be extended to include the cooling data. Other programmed
cycles that contain multiple ramps and soaks, such as actual
production drying or firing schedules, are available.
Atmospheres
For most ceramic materials, TGA tests are normally performed
in ambient air. The TG-730 and TG-740 series TGA's are
designed for ambient air or inert atmosphere operation. The
TG-720 Series are used for other controlled atmospheres,
including vacuums |