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Thermal analysis methods
03.11.06
Rolf Jentoft
Modern Methods in Heterogeneous Catalysis Research
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Outline
• Definition and overview• Thermal Gravimetric analysis• Evolved gas analysis (calibration)• Differential Thermal Analysis/DSC• Kinetics introduction• Data analysis examples
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Definition
Thermal analysis: the measurement of some physical parameter of a system as a function of temperature.
Usually measured as a dynamic function of temperature.
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– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature– DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– ...
Types of thermal analysis
– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature – DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– Combined methods
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Developed by Honda in 1915
Thermogravimetric
Oven
Balance
SampleOven heated at controlled rate
Temperature and Weight are recorded
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Types of thermal analysis
– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature– DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– Combined methods
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First introduced by Le Chatelier in 1887, perfected by Roberts-Austen 1899
DTA/DSC
Oven
Sample Reference
Oven heated at controlled rate
Temperature and temperature difference are recorded
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Types of thermal analysis
– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature– DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– Combined methods
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Dilotometry (DIL)
Dilometry: change in length with temperature
OvenPlatform
SampleLength measurement
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DIL of “Green” and SinteredYttria-stabilized Zirconia
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TMA and DMA
Thermomechanical analysis: change in sizewith temperature while under stress
Dynamic mechanical analysis: change in mechanical properties with temperature while under dynamic stress
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Glass transition starts at 75°C. The storage modulus decreased from
approx. 4,200 MPa to 200 MPa.
E‘ is storage modulusE“ is loss modulusδ is the phase lag
DMA of polyester fiber
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Types of thermal analysis
– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature – DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– Combined methods
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Dielectric analysis
Change in conductivity with temperature
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Types of thermal analysis
– TG (Thermogravimetric) analysis: weight– DTA (Differential Thermal Analysis): temperature– DSC (Differential Scanning Calorimetry): temperature – DIL (Dilatometry): length– TMA (Thermo Mechanical Analysis): length (with strain)– DMA (Dynamic-Mechanical Analysis): length (dynamic)– DEA (Dielectric Analysis): conductivity– Thermo Microscopy: image– Combined methods
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Sintering of W 1600-2700 °C
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TGA with Optical Window
Matzakos and Zygourakisa Rev. Sci. Instrum. 64 (6), June 1993, 1541-48
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TG analysis
A (Solid) B (Solid) + C (Gas)
Thermolysis curve
Pyrolysis curve
Thermogram
Thermogravimetric curve
Thermogravigram
Thermogravimetric analysis curve
TG curve
Information obtained depends on procedure Not fundamental property
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1) Thermal decomposition of substances (calcination and heat treatment and polymer stability)
2) Corrosion of metals3) Determination of moisture, volatiles, and ash content4) Evaporation rates and sublimation5) Distillation and evaporation of liquids6) Reaction kinetics studies7) Compound identification8) Heats of vaporization and vapor pressure determinations
TG analysis: uses
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TG curve: Instrumental effectsFurnace heating rate
Slower heating = better resolution
Usually, Higher heating rate =
shift to higher temperature
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TG curve: Instrumental effectsFurnace gas atmosphere
A (solid) B (solid) + C (gas)A (solid) B (solid) + C (gas)A (solid) + B (gas) C (solid)A (solid) + B (gas) C (solid)A (solid) + B (gas) C (solid) + D (gas)A (solid) + B (gas) C (solid) + D (gas)
Solid line in nitrogen,dashed line in oxygen
CaC2O4.H2O (s) CaC2O4 (s) + H2O (g)CaC2O4 (s) CaCO3 (s) + CO (g) (in N2)CaC2O4 (s) + ½ O2 (g) CaCO3 (s) + CO2 (g) (in O2)CaCO3 (s) CaO + CO2 (g)
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TG curve: Instrumental effectsFurnace gas atmosphere
CaC2O4.H2O (s) CaC2O4 (s) + H2O (g)CaC2O4 (s) CaCO3 (s) + CO (g) (in N2)CaC2O4 (s) + ½ O2 (g) CaCO3 (s) + CO2 (g) (in O2)CaCO3 (s) CaO + CO2 (g)
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TG curve: Instrumental effectsFurnace configuration
Dehydration of CaC2O4.H2O, (dashed line, single crystal)
2 K/min 8 K/min
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0 20 40 60 80 100Time /min
200
400
600
800
1000
Temperature /°C
-6
-5
-4
-3
-2
-1
0
TG /mg[2]
[2]
Carbon in 21% oxygen
0 20 40 60 80 100Time /min
200
400
600
800
1000
Temperature /°C
-6
-5
-4
-3
-2
-1
0
TG /mg
[1]
[1][2]
[2]
0 20 40 60 80 100Time /min
200
400
600
800
1000
Temperature /°C
-6
-5
-4
-3
-2
-1
0
TG /mg
[1]
[1][2]
[2]
TG curve: Instrumental effectsCorrection file
Measurements may have a significant change in weight due to changes in gas density and viscosity
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TG curve: Sample effectsCrucible type
Mass transport by flow (ΔP) and diffusion (ΔC)
Gas Flow
A (solid) B (solid) + C (gas)A (solid) + B (gas) C (solid)A (solid) + B (gas) C (solid) + D (gas)
•Thin layer vs. Large amount of sample
•Detection limit vs. Diffusion limitation
•Self generated atmosphere
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TG curve: Sample effectsThermal conductivity and particle size
Large particles and low thermal conductivity can effect results
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Combustion of carbon, combind TG/DSC
0 20 40 60 80 100Time /min
0
50
100
150
200
DSC /uV
200
400
600
800
1000
Temperature /°C
20
40
60
80
100
TG /%
[4]
[4]
[4]
↑ exo
TG curve: Sample effectsDiffusion limitation
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Evolved gas analysis
•Single thermal analysis method may not be sufficient to understand changes in sample
•Control of gas phase requires analysis of gas phase
•Mass spectrometry and Infra-red analysis
•Transfer of gas to analytical instrument
•Calibration of the gas analysis technique
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Evolved gas analysis: Pulse Calibration
Inject known volume of gas into TG under measurementconditions
Integrate peak in MS
Response factor is moles gas divided by area of peak
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Thermal analysis: crucibles
The best type of crucibles are disposable crucibles
Crucible selection criteria (size and material):
Temperature rangeChemical compatibilityDetection limitsGas exchange characteristics
Crucible cleaning
Mechanical cleaning not recommended
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Thermal analysis: crucibles
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DTA/DSC
Measure temperature difference between sample and reference while they are being heated.
Measure difference in heat flow to sample and reference while they are being heated.
DTA DSC
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DSC
Heat flux DSC Power compensating DSC
•Heat flows through disk•Temperature of disk measured•Heat transfer through disk greater
than through gas phase
•Each sample has own heater•Temperature of samples controlled
independently•Less power required with endotherm
Sample Reference
oven
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DSC
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DTA/DSC :Reference
Reference should have same physical properties as sample
Reference should not have any transformations during heating
Reference for sample which looses weight?
Commonly used, SiC, Al2O3, empty crucible
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DTA/DSC: Temperatures
Temperature of oven, reference and sample during measurement
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Heat integration
Curing a epoxy resin,Simple linear baseline
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Heat integration
Re-heat cured resin to measure baseline (heat capacity) at end of reaction
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TG analysis: combined methods
Thermal analysis methods are more powerful when combined
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Analysis Methodology
• VxOy Characterization
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• Model catalyst for partial oxidation of butane– Alkoxide/benzyl alcohol route*
• Catalytic properties– At 473 K mainly acetic acid
(C-C bond clevage)– At 573 and 673 K mainly malaic anhydride
(oxidation)• Previous knowledge
– From EELS and XPS V oxidized from mix of V+3
and V+4 to V+4 and V+5
VxOy Nanoparticles
N. Pinna, M. Antoneitti, M. Niederberger, Colloids Surf. A 250 (2004) 211.
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• From TEM, EELS, and XPS vanadium is oxidized from V+3 and V+4 to V+4 and V+5
• What causes the change in selectivity?
• What can TGMS tell us about the material?
• Only several milligrams of material available!
VxOy Nanoparticles
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0 20 40 60 8090
92
94
96
98
100
Tem
pera
ture
, °C
Wei
ght,
%
Time, min
0
100
200
300
400
500
TGMS of VxOy particles
0 20 40 60 8090
92
94
96
98
100
Ion
Cur
rent
,A
mps
Tem
pera
ture
, °C
Wei
ght,
%
Time, min
0.02.0x10-104.0x10-106.0x10-108.0x10-101.0x10-91.2x10-91.4x10-91.6x10-91.8x10-92.0x10-92.2x10-9
M/e 18 M/e 44
0
100
200
300
400
500
Conditions: 21 % oxygen, 5 K/min to 773K
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0 20 40 60 8090
92
94
96
98
100
Tem
pera
ture
, °C
Mas
s, %
Time, min
M/e 18 M/e 44
0
100
200
300
400
500
• Calibrate MS:– H2O (CuSO4*4H2O) – CO2 (pulse valve)
• First M/e 18: 0.94mg
• Dehydration and combustion (assume C:H = 1:1) = 1.92 mg• Weight loss of only 1.77mg suggests simultaneous re-
oxidation• Prolonged re-oxidation produces V2O5: basis for valence
calculation of 4.5 at 340°C.
TGMS of VxOy particles
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References
G.W.H. Höhne, W.F. Hemminger, H.-J. Flammersheim, Differential Scanning Calorimetry, Second edition, Springer, Berlin, 2003
W.W. Wendlandt, Thermal Methods of Analysis, John Wiley & Sons, New York, 1974
W.F. Hemminger, H.K. Cammenga, Methoden der ThermischenAnalyse, Springer-Verlag, Berlin, 1989
T. H. Gouw, Guide to Modern Methods of Instrumental Analysis,Wiley-Interscinece, New York, 1972
H.H. Willard, L.L. Merritt, Jr., J.A. Dean, F.A. Settle, Jr. Instrumental Methonds of Analysis, 7th edition, Wadsworth, Belmont, 1988
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Acknowledgement for Examples
Max Planck Institute for Colloids and Interfaces
Markus Antonietti Matthijs Groenewolt Nicola PinnaMarkus Niederberger
Fritz-Haber-Institute of the MPG, Department of Inorganic Chemistry
Robert SchlöglAnnette TrunschkeMichael HäveckerDangsheng SuDi WangKlaus WeissUte WildJuan Delgado (diffusion limited combustion example)
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Ice Calorimeter by Lavoisier
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