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 CaO
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
 TiO(Oxinate)2. xH2O TiO(Oxinate)2 TiO2

TG and DTA curves for Zn Oxinates precussor precipitate

% Weight loss
Therotical Experiment

1st 9.2 8.2

2nd 79.9 82.7
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) 650
Pb(Zr0.52TiO0.48)O3
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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