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STUDIES ON THERMAL DECOMPOSITION OF SOME MIXED METAL OXINATES

STUDIES ON THERMAL DECOMPOSITION OF SOME MIXED METAL OXINATES CHAPTER

–I

INTRODUCTION

CHAPTER – II

LITERATURE SURVEY & RESEARCH OBJECTIVES

CHAPTER – III

EXPERIMENTAL 3.1 Sample Preparation (A) Oxinates of Mg, Mn, Zn, Ni, Ca, La, Bi, Zr, Ti, Pb, W, Fe (B) Pb-Ti, Pb-(Zr, Ti) and Bi-Ti oxinates (C) M-Fe Oxinates (M=Mg, Mn, Zn, Ni) 3.2 Characterization Techniques

CHAPTER – IV

RESULTS AND DISCUSSION

4.1 Oxinates of Mg, Mn, Zn, Ni, Ca, La, Bi, Zr, Ti, Pb, W, Fe 4.2 Pb-Ti, Pb-(Zr, Ti) and Bi-Ti oxinates 4.3 M-Fe Oxinates (M=Mg,Mn,Zn,Ni) 4.4 CONCLUSIONS

• • • • •

Unit cell of Perovskite Unit cell is Tetragonal (a=b≠c, α=β=γ=90) Ba is 12 Coordinated Ti is 6 Coordinated Number of formula units per unit cell is 1

Unit cell is Cubic General formula AB2O4 A- 4 Coordinated B-6 Coordinated Number of formula units per unit cell is 8

Table : 1

Conditions used for the synthesis of metal oxinates :

S.NO

Compound

pH maintained

Metal :Oxine ratio

1

Zn-Oxinate

5.0

1:3

2

Ni - Oxinate

5.0

1:3

3

Pb - Oxinate

9.4

1:3

4

Ca- Oxinate

9.4

1:3

5

Ti- Oxinate

5.4

1:6

6

Fe- Oxinate

4.6

1:10

7

Mg- Oxinate

9.5

1:3

8

Mn- Oxinate

9.5

1:3

9

Bi- Oxinate

5.6

1:10

10

Zr - Oxinate

9.4

1:6

Metal ion solution = 0.1M Oxine =0.2M in Acetic acid

S.NO

Compound

pH maintained

1

Pb-Ti Oxinate

8.5

2

Pb (Zr, Ti) Oxinate

9.1

3

Bi-Ti Oxinate

5.8

S.NO

Compound

pH maintained

1

Zn-Fe Oxinate

5.1

2

Ni-Fe Oxinate

5.2

3

Mn-Fe Oxinate

9.0

4

Mg-Fe Oxinate

9.3

TG and DTA curves for Zn Oxinates precussor precipitate % Weight loss Therotical Experiment Reaction Type 1st Loss 9.24 9.30 Loss of water 2nd Loss

79.1

81.5

Decomposition

XRD Corresponds to Zinc Oxide phase

2Fe(Oxinate)3

Fe2O3

TG and DTA curves for Iron Oxinate Precussor precipates % Weight loss Theoretical Experimental 83.6 83.7

XRD Corresponds to Ferric Oxide phase

Pb(Oxinate)2

PbO

TG and DTA curves for Lead Oxinate Precussor precipates % Weight loss Theoretical Experimental 54.9 54.4

XRD Corresponds to Lead Oxide phase

Ca(Oxinate)2.2H2O

Ca(Oxinate)2

CaCO3

TG and DTA curves for Ca Oxinate Precussor precipates % Weight loss Theoretical Experimental 1st 9.89 11.6 2nd 73.5 74.8 3rd 84.6 87.4

CaO

TiO(Oxinate)2. xH2O

TiO(Oxinate)2

TG and DTA curves for Zn Oxinates precussor precipitate % Weight loss Therotical Experiment 1st 2nd

9.2 79.9

8.2 82.7

TiO2

XRD Corresponds to Titanium Oxide phase

Mn(Oxinate)2

MO

TG and DTA curves for Manganese Oxinate Precussor precipates % Weight loss Theoretical Experimental 76.8 82.0

XRD Corresponds to Manganese Oxide phase

2La(Oxinate)3

La2O3.CO2

La2O3

TG and DTA curves for La Oxinate Precussor precipates % Weight loss Theoretical Experimental 67.6 69.4

WO2(Oxinate)2

WO2C2O5.CO2

WO3

TG and DTA curves for W Oxinate Precussor precipates % Weight loss Theoretical Experimental 1st 27.8 29.0 2nd 53.98 56.4

2ZrO2.3(Oxinate)

ZrO2

TG and DTA curves for Zr Oxinate Precussor precipates % Weight loss Theoretical Experimental 69.0 62.7

XRD Corresponds to Zirconium Oxide phase

Ni(Oxinate)2.2H2O

Ni(Oxinate)2

NiO

TG and DTA curves for Ni Oxinate Precussor precipates % Weight loss Theoretical Experimental 78.48 80.9

XRD Corresponds to Nickle Oxide phase

Mg(Oxinate)2

MgO

TG and DTA curves for Magnesium Oxinate Precussor precipates % Weight loss Theoretical Experimental 73.0 68.0

XRD Corresponds to Magnesium Oxide phase

Bi

Bi(Oxinate)

Bi2O3

TG and DTA curves for Bi Oxinates precussor precipitate % Weight loss Therotical Experiment 46.5

47.0

XRD Corresponds to Bismuth Oxide phase

Pb(Oxinate)2+TiO(Oxinate)2.xH2O

650

PbTiO3

Pb(Oxinate)2+0.52ZrO2(Oxinate)1.5+0.48TiO(Oxinate)2.H2O) Pb(Zr0.52TiO0.48)O3

650

4Bi(Oxinate)+3TiO(Oxinate)2.2H2O

700

Bi4Ti3O12

Mg(Oxinate)2+2Fe(Oxinate)3

900

MgFe2O4

Ni(Oxinate)2.2H2O+2Fe(Oxinate)3

900

NiFe2O4+(NiO+Fe2O3)

Zn(Oxinaate)2.2H2O+2Fe(Oxinate)3

900

ZnFe2O4

Mn(Oxinate)+2Fe(Oxinate)3

900

MnFe2O4

CONCLUSIONS Based on the experimental results it may be concluded that • The present proposed method of making use of oxinates as the precursors is useful for synthesing PbTiO3, Bi4Ti3O12 and Mg FeO4. • For other mixed metal oxides the temperatures of investigation were not sufficient for pure phase PZT, NiFe2O4, MnFe2O4 and ZnFe2O4. • Some more work is needed to establish the synthesis Conditions of the above mixed metal oxinates.

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