THERMAL ANALYSIS OF METAL IMPREGNATED SOL-GEL ALUMINA GRANULES

THERMAL ANALYSIS OF METAL IMPREGNATED SOL-GEL ALUMINA GRANULES.  
 
 
 

Thermal analysis is measurement and interpretation of the relationship between the physical/chemical properties of sample and temperature.  Temperature of sample is controlled in a predetermined way-either by continuously increasing or decreasing the temperature at constant rate (linear heating or cooling) or by carrying out a series of determinations at different temperatures (Isothermal measurements).

Thermal analysis is a good tool to measure thermal decomposition of solids and liquids, solid-solid and solid-gas chemical reactions and phase transitions.  Thermal analysis is done using various methods and these methods are distinguished from one another by the property by which they are measured.

1. Differential Thermal Analysis (DTA): Temperature difference
2. Differential Scanning Calorimetry (DSC): Heat difference
3. Thermogravimetric Analysis (TGA): Mass
4. Thermo Mechanical Analysis (TMA): Dimension
5. Evolved Gas Analysis (EGA): Gaseous decomposition products

The parameter (temperature) for calcination process of sol-gel alumina granules is optimized using DTA and TGA. 
 
 
 

THERMOGRAVIMETRIC ANALYSIS (TGA)

TGA is the branch of thermal analysis which examines the change in mass of a sample as a function of temperature.   The change in mass is observed due to the evolution of gases from the sample.  Nitrogen gas is used here. 
 

           Figure 1: Thermogravimetric analyzer (TA-2050) 
 
 
 
 
 
 

      Figure 2: Blow-up of sample loader 


Precise measurement of weight change of solid is useful to determine sample purity, water, organic content and for study of decomposition reactions.

Data from TGA-2050 was acquired using the following procedure.

1. Turn on the TGA-2050 and then the computer.
2. Click on the TA thermal solution icon and then Thermal solutions instrumental control.
3. Go to method editor and then segment types.
4. In segment types the following data was given:
 


Equilibrate at 30C.

Ramp 10C/min to 500C.

Isothermal for 1 min (Maintains temperature at 500C for 1 min).

Ramp 10C/min to 30C.

Isothermal for 1 min (Maintains temperature at 30C for 1 min).

Data storage: On.

   The above method was saved.

5. Tear the pan weight and then put the sample whose weight is known.
6. Sample details were given in experiment parameters and then method was loaded.

As temperature of sample was raised, chemical reactions occurred resulting in change of sample weight.  Change in weight was measured as a function of temperature.  The following trend is observed. 


                  dm

Temperature

      Figure 3: General trend of sample in TGA (weight change versus temperature)

TGA curve provides information about thermal stability of initial sample, intermediate compounds formed and also that of residue. 
 
 


DIFFERENTIAL THERMAL ANALYSIS (DTA)

DTA involves heating of sample and reference under identical conditions, while recording temperature difference between sample and reference.  This differential temperature is then plotted against time or temperature.  DTA determines the precise temperature at which reaction takes place or identifies phase change.

The DTA used here is DTA-50.  DTA-50 consists of an insulated chamber (furnace) containing a reference pan, sample, heater and two thermocouples. 
 
 

Figure 4:

alyser (DTA-50) 
 
 

        Reference           Sample                                  Heating Coil

                            Gas                  Thermocouples

Figure 5: Schematic Diagram of DTA 

Following procedure was used to acquire data from DTA-50.

1. Turn on the DTA-50 and then the TA-60WS.

   2. Open the compressed air and water valves.
   3. Switch on the control of the blower and then the computer.

   Press

   5. Load the sample on right side pan after the furnace shifts upwards, the left side pan being for the reference (Pans like aluminium, platinum are sued based on the temperature maintained).
   To  move furnace down press

   7. Click the TA-60WS icon the computer screen and select DTA-50, TA-60 Ch.1 (detects the signal).

      8. Select measure, give file information, temperature program (temperature increase per min) and then upload.
      9. Click start either on the screen or on the DTA-50 apparatus.

      Interpretation of data obtained from DTA-50.

      Temperature of both sample and reference were raised slowly from room temperature to 475C using furnace heater.

      The reference has no phase transitions within the heating range and was heated linearly.

            

      Temperature 
      

        

       
       
       
       
       
       
       
      

            

      Time 
       
      

        Figure 6: Temperature versus time showing no transition in reference temperature 
       
       
      

      The baseline of DTA curve exhibited discontinuity at transition temperature that is the temperature of sample deviated from temperature of reference.  This te

      mperature difference was detected, amplified and recorded as a peak. 
      

                            Temperature                           

                                                         

          Time 
      

             

      Figure 7: Temperature versus time showing phase transitions of a sample 
      

      The peak lower than baseline represents melting transition and peak above baseline represents glass transition.

      For all the granules with different compositions of metal the following similar trend was observe

      d.  At 100

      

      C a peak (arrow pointed upwards in figure was observed.  This peak represents removal of water from the granules.  The incomplete peak at 475

      

      C indicates that melting point of granules is greater than 475

      

      C, showing that granules can be calcined

      at 450

      

      C.

        
      

                Temperature

              Time

      Figure 8: Temperature versus time graph showing variation in temperature profile

                       of sol-gel alumina granules. 
      

      CONCLUSION

      DTA compares the difference between sample and reference as a function of temperature resulting in values of phase transition temperature.  TGA compares the mass change of sample as a function of temperature giving the sublimation temperature.  Thus with DTA and TGA the metal impregnated sol-gel alumina granules could be calcined at 450C.

      REFERENCES

      1. Differential thermal analysis – Smothers W. J.

      2. http://www.users.globalnet.co.uk/~dmprice

         3. http://www1.shimadzu.com
         4. Thermal analysis of materials – Speyer, Robert F.
         5. Differential thermal analysis of lunar soil stimulant – Tucker D.
         6. www.binghamton.edu