FINAL YEAR PROJECT 2

(Semester1, Academic Year 2008/2009)

Title : Sintering Behaviour of

Cerium-doped
Hydroxyapatite Bioceramics

Prepared by:
KELVIN HOH CHEE WAI (ME075719)
Department of Mechanical Engineering
Project Supervisor: Universiti Tenaga Nasional (UNITEN)
Assoc. Prof. Ir. Dr. Ramesh Singh
 CONTENTS

• Introduction
• Objective
• Methodology
• Experimental techniques
• Experimental testing methods
• Results & Discussions
• Conclusion
 INTRODUCTION
• Hydroxyapatite (HA), Ca10(PO4)6(OH)2, exhibits
excellent biocompatibility due to its chemistry
similarity with the mineral portions of hard tissues.

• However, its mechanical properties limit the usage

of HA in clinical application.

• Several approaches have been proposed to

improve the mechanical properties of HA, such as:
 INTRODUCTION

Control of sintering temperature & atmosphere.

Manipulation of processing parameters.

Addition of sintering additives (i.e. dopants) into

the HA powder.
 OBJECTIVE

• To investigate the effects of adding small

amounts of Cerium Oxide (CeO 2 ) on the
sinterability of nanocrystalline HA powder.
 METHODOLOGY

Literature Review FYP 1

Preparation of Cerium-doped
HA powder
Powder Characterization

Body Preparation
FYP 2
Consolidation Process

Mechanical Testing & Evaluation

Report preparation & presentation

 Experimental Techniques
• Synthesized HA powder which is produced by wet chemical
precipitation method was used and mixed with CeO2 ranging
from 0.1 wt% - 1.0 wt% using wet milling method.

• The powder was uniaxially pressed into discs and rectangular

bars and subsequently cold isostatically pressed at 200 MPa.

• The compacted samples were sintered at temperature ranging

from 1100C to 1300C.

• Sintered samples were polished to 1m finish prior to testing.

Experimental Testing Methods

• Phase analysis  X-Ray Diffraction (XRD).

• Bulk density  Water Immersion Technique.

• Young’s modulus  Sonic Resonance Method.

• Hardness  Vicker’s Indentation Method.

• Fracture Toughness  Vicker’s Indentation Method.

 RESULTS & DISCUSSIONS
(XRD Analysis)

• XRD analysis revealed that

Ceria Peaks @ 1 wt% the doped & undoped HA
phase stability were not
dis r upt ed r egardless of
dopant additions and
sintering temperature.

Fig 1: XRD patterns for CeO2-doped HA sintered at 1300 C.

(a) undoped HA, (b) 0.1 wt%, (c) 0.5 wt%, (d) 1.0 wt%
CeO2, respectively.
 BULK DENSITY

• In general, the bulk density

3.14 variation of all the composition
studied exhibited a similar
Bulk Density (g/cm 3)

3.13
trend with increasing sintering
3.12 temperature.
3.11
0wt%
0.1wt% • All the samples attained above
3.1
0.5wt%
1.0wt%
98% of theoretical density
3.09 when sintered above 1100ºC.
1100 1200 1300

Sintering Tem perature (ºC)

Fig 2: The effects of CeO2 addition on the bulk density of

synthesized HA.
 YOUNG’S MODULUS

126
• The relationship between the
125 Young’s modulus of the
Young's modulus (GPa)

124 undoped
sintered body, sintering
123 0.1 wt% temperature and CeO2
122
0.5 wt% additions are shown in Fig 3.
1.0 wt%
121
120
119 • The inclusion of CeO2 in HA
118
117 reduces the Young’s modulus.
1050 1100 1150 1200 1250 1300 1350
Sintering Tem perature (°C)
• However, the Young’s
Fig 3: The effects of CeO2 addition on the Young’s modulus modulus of natural bone is
of synthesized HA. reported to be between 11
GPa to 29 GPa.
 YOUNG’S MODULUS

Fig 4: Fracture toughness versus Young’s modulus of present biomaterials and human bone.
 VICKER’S HARNESS
• A general observation shows
7
measured hardness of all the
samples revealed a similar
6
trend.
Hardness (Gpa)

5
4
• The results also revealed that
undoped
3 the addition of 1 wt% CeO2
0.1wt%
2
0.5wt%
was beneficial as samples
1 1.0wt% exhibited higher hardness
0 value in the sintering regime
1100 1200 1300 employed as compared to
Sintering Temperature (°C)
undoped HA.

Fig 5: The effects of CeO2 addition on the Vicker’s Hardness • The highest hardness value of
of synthesized HA. 6.19 GPa was obtained for HA
doped with 1 wt% CeO2 and
when sintered at 1200ºC.
 FRACTURE TOUGHNESS
• The results also show that the
addition of CeO2 was effective
Fracture Toughness (MPam1/2)

0.9
0.8 in enhancing the fracture
0.7
0.6 toughness (KIc) of the
0.5 synthesized HA, particularly
0.4 Undoped
0.3 0.1wt%
when sintered at 1100ºC.
0.2 0.5wt%
0.1 1.0wt%
0 • The 1 wt% cerium-doped HA
1100 1200 1300
samples exhibited the highest
Sintering Temperature (°C) fracture toughness of 0.82
Fig 5: The effects of CeO2 addition on the fracture toughness MPam1/2 as compared to 0.73
of synthesized HA. MPam1/2 measured for the
undoped HA.
 CONCLUSIONS

• Incorporation of small amount of cerium oxide can be

beneficial in enhancing the mechanical properties without
affecting the HA phase stability even when sintered at
1300ºC.

• The addition of 1 wt% CeO2 and when sintered at 1100ºC

was found to be most beneficial as the HA samples
exhibited the moderate Young’s modulus of 120.53 GPa,
enhanced hardness of 6.19 GPa and fracture toughness of
0.82 MPa.m1/2.
FURTHER WORK SUGGESTIONS