Two step sintering of a novel calcium magnesium silicate bioceramic:
Sintering parameters and mechanical characterization
Ali Nadernezhad
a
, Fathollah Moztarzadeh
a,∗
, Masoud Hafezi
b,∗∗
, Hadi Barzegar-Bafrooei
c
a
Biomaterials Group, Faculty of Biomedical Engineering (Center of Excellence), Amirkabir University of Technology, P.O. Box 15875-4413, Tehran, Iran
b
Biomaterials Group, Nanotechnology and Advanced Materials Department, Materials and Energy Research Center, P.O. Box 31787-316, Karaj, Iran
c
Ceramic Division, Materials and Energy Research Center, P.O. Box 31787-316, Karaj, Iran
Received 31 October 2013; received in revised form 2 May 2014; accepted 8 May 2014
Available online 28 May 2014
Abstract
Two-step sintering (TSS) was applied to control the grain growth during sintering of a novel calcium magnesium silicate (Ca
3
MgSi
2
O
8
– Merwinite)
bioceramic. Sol–gel derived nanopowders with the mean particle size of about 90 nm were sintered under different TSS regimes to investigate the
effect of sintering parameters on densification behavior and grain growth suppression. Results showed that sintering of merwinite nanopowder
under optimum TSS condition (T
1
= 1300
◦
C, T
2
= 1250
◦
C) yielded fully dense bodies with finest microstructure. Merwinite compacts held at
T
2
= 1250
◦
C for 20 h had the average grain size of 633 nm while the relative density of about 98% was achieved. Mechanical testing was performed
to investigate the effect of grain growth suppression on the hardness and fracture toughness. Comparison of mechanical data for samples sintered
under two sintering regimes, including TSS and normal sintering (NS), showed TSS process resulted in significant enhancement of fracture
toughness from 1.77 to 2.68 MPa m
1/2
.
© 2014 Elsevier Ltd. All rights reserved.
Keywords: Two-step sintering (TSS); Merwinite; Mechanical properties; Sinterability
1. Introduction
During the past two decades, many researchers have shown
interest on development of novel processes and techniques to
produce nanostructured synthetic ceramics. These efforts have
mainly focused on using novel synthesis methods as well as
improved processing techniques. Sintering, as an important
stage in ceramics processing, has also undergone significant
modifications and some novel sintering routs were introduced.
Since vast microstructural changes occur during sintering,
the main goal of these novel techniques was to control the
microstructural features of ceramics like grain size and density.
∗
Corresponding author. Tel.: +98 21 64542393; fax: +98 21 64542393.
∗∗
Corresponding author. Tel.: +98 26 36280040 9; fax: +98 26 36201888.
E-mail addresses: a.nadernezhad@aut.ac.ir (A. Nadernezhad),
moztarzadeh@aut.ac.ir (F. Moztarzadeh), mhafezi@merc.ac.ir,
masoud.hafezi@gmail.com (M. Hafezi), hadi.merc@gmail.com
(H. Barzegar-Bafrooei).
Using of sintering additives was reported as a successful method
to control grain growth during sintering.
1–4
However, there are
some limitations and disadvantages for using of a second phase
particles due to the possible adverse effects on physical and
chemical properties. Many researchers reported successful uti-
lization of pressure and extremely high rates of heating during
sintering like hot pressing (HP),
5
spark plasma sintering (SPS)
6
and microwave sintering (MWS).
7
The main aim of these non-
conventional sintering methods was shortening the heating time
to hinder the grain growth. However, the application of pressure
and also high rates of heating would be costly and needs special
equipment.
A new approach which has been introduced by Chen and
Wang
8
is to suppress the grain growth during final stage of sin-
tering, by taking advantage of the difference between required
energy for migration of grain boundaries and the activation
energy required for diffusion of mater through grain boundaries.
The simple nature of this promising method, which is called two-
step sintering (TSS), made it attractive for many researchers