To analyse the structure of Ca doped ZrO2

By

U Sri Guna Kaushik-2015B2AB0708H

INTRODUCTION:

Zirconium oxide (Zirconia) is a white crystalline oxide of Zirconium, naturally occurring with a
monoclinic structure.

This report helps us to find out the structure of Calcium doped Zirconium oxide. Generally,

when we dope small amount of calcium to Zirconia, we have two possibilities of calcium atom

settling in the lattice of Zirconia i.e, Ca atom going to the interstitial void of Zirconia lattice or

Ca atom occupying the lattice positions changing the whole lattice structure.

METHODS AND MATERIALS:

The method used for the synthesis of CaxZr1-xO2-y is microwave synthesis. The precursor

materials used for the synthesis are Calcium carbonate and Zirconia. Due to unavailability of

Zirconia in the lab, it was prepared by precipitating the Zirconium oxycholride (ZrOCl2).

Zirconium oxychloride was dissolved in water and treated with NaOH to increase the pH of the

solution. The solution was then washed with water and calcined to get dry Zirconia.
The Zirconia and Calcium carbonate were grinded in a mortar homogenously. The homogeneous

mixture was taken in 8% PVA solution and put in microwave oven exposing it to the

microwaves. The Zirconia being non responsive to the microwave till 400°C, we use PVA

solution as a catalyst to increase the mixture temperature to the required level there by providing

the condition for the mixture to react. [1]

RESULTS AND DISCUSSION:

To check the presence of Na in ZrO2 and Ca in  CaxZr1-xO2-y X-ray Fluorescence (XRF) was

performed.

The XRF plot of ZrO2

We performed XRF for Zirconia is to detect the presence of Na as we added NaOH to dissolved

Zirconium oxychloride to increase the pH. From the above plot, we can say that the presence of

Na hasn’t occurred.
The XRF plot of CaxZr1-xO2-y
From the above XRF plot, we have confirmed the presence of Ca in the final mixture (product).

Meas. data:Mixture Ca ZrO2

1000
Intensity (cps)

500

20 30 40 50 60 70 80
2-theta (deg)

XRD plot for CaxZr1-xO2-y

Peaks list of above XRD plot

From the above XRD plot, we can say there are multiple phases according to the peaks obtained.

This occurred due to the low temperature synthesis of CaxZr1-xO2-y (limitation in our microwave

synthesizer) and also due to non homogenous mixing of the calcium carbonate and the Zirconia

resulting in some of the Zirconia left unreacted. In the above XRD plot we find the multiphase of

cubic structure at (111), (200), (220), (311), (222), (400) and other peaks corresponding to the

unreacted monoclinic structure of the Zirconia.

CONCLUSION:

The observed cubic structure from the XRD of CaxZr1-xO2-y concludes the formation of different

lattice structure from monoclinic structure of Zirconia. If the Ca atom settles in the interstitial

void of Zirconia, the final product should not contain peaks corresponding to other 2-theta

values, thus confirming the change in structure of Zirconia.

REFERENCES:

[1] Anirudh P. Singh,W Navdeep Kaur, and Ajay Kumar, “Preparation of Fully Cubic Calcium-Stabilized

Zirconia With 10 mol% Calcium Oxide Dopant Concentration by Microwave Processing”, Journal of the

American Ceramic Society—Singh et al. Vol. 90, No. 3.