Available online at www.sciencedirect.com
Journal of the European Ceramic Society 33 (2013) 629–635
Short communication
A simple approach to observe non-conductive hydrated materials with
FE-SEM: Case study on porous hydroxyapatite green bodies
Chisato Takahashi
a
, Deepak K. Pattanayak
a,b
, Takashi Shirai
a
, Masayoshi Fuji
a,∗
a
Advanced Ceramics Research Center, Nagoya Institute of Technology, 3-101-1, Honmachi, Tajimi, Gifu 507-0033, Japan
b
CSIR-Central Electrochemical Research Institute, Karaikudi, Tamilnadu 630006, India
Received 10 July 2012; received in revised form 23 September 2012; accepted 5 October 2012
Available online 28 November 2012
Abstract
The purpose of this study is to develop a simple method to observe the surface morphology of non-conductive material in its hydrated condition. Here
porous hydroxyapatite (HAp) green body prepared by gelcasting process was considered as a case study, and, the resultant body was subsequently
treated with hydrophilic ionic liquid (IL). The surface morphology and the pore structure of the IL-treated porous HAp green body were successfully
observed even in hydrated condition without any charging using field emission scanning electron microscope (FE-SEM). Results showed that the
pore diameter from 300 to 600 m in as-prepared green body was reduced to 100–300 m in the sample sintered at 1000
◦
C. Raman results showed
that the IL forms weak hydrogen bond with water molecules within the sample and, that prevents from drying in vacuum condition. In addition,
the IL acts as a conducting media for HAp ceramics to be observed under FE-SEM.
© 2012 Elsevier Ltd. All rights reserved.
Keywords: Ionic liquid; Gelcasting; Hydroxyapatite; Hydrated materials; FE-SEM
1. Introduction
Room temperature ionic liquid (RTIL) ([emim][BF
4
]) was
reported in 1992. Since then, ionic liquids (ILs) have gained
popularity among the researchers due to their unique properties
such as non-volatile, non-flammable, chemical/thermal stability
and high conductivity.
1–4
These ILs are composed of asymmet-
rically substituted organic cations with anions, and, remained as
fused salts at room temperature. Most significantly, the ILs with
different combinations of cations and anions affect the properties
such as polarity, melting point, hydrophilicity and hydropho-
bicity. Therefore, the IL properties can be adjusted to suit the
requirements of a particular process.
The ILs are widely used in bio-materials and agro-materials
to improve the properties such as compatibility and thermal sta-
bility, etc.
5,6
In addition, formation of conductive polymer using
the IL showed useful applications especially in the field of life
sciences.
7–10
The ILs are also used as solvents in various chem-
ical reactions, or in dispersion of carbohydrate polymers such
∗
Corresponding author. Tel.: +81 572 24 8110; fax: +81 572 24 8109.
E-mail address: fuji@nitech.ac.jp (M. Fuji).
as cellulose and starch, etc. Besides, composite gel mixed with
the IL is used in drug delivery as well as fabrication of contact
lenses.
11–14
Recently, alkylimidazolium ILs such as alkylimida-
zolium tetrafluoroborates and hexafluorophosphates have shown
promising lubricating properties as base oils for a variety of
contacts.
15–18
The ILs are also used for fabricating good solid
electrolytes for safer lithium batteries.
19–21
Besides above mentioned applications, due to negligible
vapor pressure coupled with high conductivity, specimens
treated with the IL is used in various electron microscopic obser-
vations (SEM/TEM) under vacuum conditions.
22–31
Kuwabata
et al. initially proposed the application of IL for observation
of biological sample using SEM. Later on, several research
groups reported that biological materials such as human cul-
ture cells, fungal, chicken tissues and other biological samples
can be observed in SEM under vacuum. Most recently, present
authors also proposed that agar gel which is a hydrated material
can be observed in FE-SEM when it is previously treated with
the IL solution.
29–31
Although some reports suggest the suitabil-
ity of IL for microscopic observation, still this method is limited
to few kinds of materials.
In the present study, a simple method of microstructure obser-
vation of hydrated ceramic materials is attempted. In order to
0955-2219/$ – see front matter © 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jeurceramsoc.2012.10.037