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Preparation of Hydroxyapatite Scaffold using

Luffa cylindrica Sponge as Template


Ahmad Fadli, Heni Ismawati
Department of Chemical Engineering, University of Riau, Riau, Indonesia
Kampus Binawidya Km 12,5 Simpang Baru Panam, Pekanbaru 28293
fadliunri@yahoo.com; Tel: +628126613521

1. Introduction
Nowadays, hydroxyapatite (HA) scaffold has been widely applied in the biomedical
field especially for bone implants. For biomedical bone implant pores system even
necessaries to cell growth area. The ideal HA scaffold is a material that has pores system
which form a secure bond with the tissues, increasing the mechanical fastening between
an implant and bones [Swain et al, 2015]. One way to achieve this pores system that use
template as in polymeric sponge method [Sopyan dan Kaur, 2009].The main advantage of
this technique is, that HA scaffold has very good interconnected pores [Dobo, 2012]. HA
Scaffold should has interconnected pore structure with high porosity. The pore diameter
are about above 300 microns for penetrating the cell, tissue growth, and vascularization
[Barbara, 2005].
Luffa cylindrica is a kind of tropical plant and the vine of the family cucurbitaceae
[Tanobe et al, 2005]. It has microcellular architecture fibers that form net-like fibrous
vascular system. The struts of Luffa cylindrical sponge which has 200-400 m diameter
form by microcellular architecture macro-pore with diameter of 1020 m and yield a
multimodal hierarchical pore system that can be using as a template in the manufacture of
porous material [Zampieri et al, 2006].
Sopyan and Kaur [2009] have pointed out in their investigation based on amount
of solid loading HA. HA scaffold has been made by polymeric-sponge method
using commercial cellulose (Spontex Spa, Italy), dispersant 3% of solid loading
HA, sintering temperature 1200oC for an hour. Solid loading HA amount are
38%w; 42%w; and 44%w. The result indicated an addition of 42%w solid loading
produced HA scaffold with density 2.08 g/cm3 and compressive strength 10.5 MPa.
Jamaludin et al [2015] produced HA scaffold using commercial polyurethane sponge
(20 pore/inci, CCT Automation Sdn Bhd). HA scaffold has been fabricated based on
influence of binder type (PVA, sago starch and tapioca). The result shows that sago starch
produced highest density is 0.83 g/cm-3.
Fu et al [2008] have done their research to producing HA scaffold by freeze-casting
method based on type of dispersant (Darvan C, Darvan 811, Darvan 812A, Targon 1128).
The result shows darvan 821A usage producing 55% of good structure porous.
This work focuses on the preparation hydroxyapatite scaffold using luffa cylindrica
sponge, which amount of solid loading HA and darvan 821A were varied. This method is
using a template to form macroporous ceramics by impregnation cell structure with
ceramic suspense to produce similarity morphology as well as template, where the
ceramic suspense be made by varied solid loading and dispersant.

2. Experimental Procedure
2.1 Raw Materials
The pure HA powder as solid loading was supplied by Lianyungang Kede
Chemical Industry co. Ltd, China. Luffa cylindrica sponge as template was supplied by
Trendy, Indonesia. Sago starch as binder supplied by Puri Pangan Sejahtera, Indonesia.
Darvan 821A as dispersant supplied by Vanderbilt Company, USA. And distilled water
as solvent was supplied by Brataco Chemica, Indonesia.

2.2 Template Preparation


Porous template prepared by soaking Luffa cylindrica sponge for 12 hours in
order to make it expands. Sponges were cut into circular samples of 10 mm diameter
then dried in the open air for an hour.

2.3 Slurry Peparation


The slurries were prepared by dissolving 10, 11 and 12 g hydroxyapatite powder
with 10 g sago starch, 2%; 2.5%; and 3% Darvan 821A and 12 g distilled water. The
slurries was stirred using magnetic stirrer with rate of 350 rev min-1 for 20 hours. The
sponges then impregnated with the slurry and dried using an air oven at 110 oC for 3
hours. The organic matrix are eliminated through burning process using a muffle
furnace at 600oC for 1 hour and followed by sintering at 1250oC for 1 hour.

2.4 Characterization of HA scaffold


The percentage of shrinkage was calculated based on the difference in scaffolds
volume before and after sintering. Scaffolds porosity is obtained through the
calculation of density and relative density. Morphology scaffolds analyzed by SEM.
Compressive strength of scaffolds obtained from analyzed using Universal Testing
Machine.

3. Result and Discussion


3.1 Body Properties of HA scaffold
Polymeric-sponge method is a methods to achieve pores structures of
scaffold HA has similarity as good as the template. This work is using Luffa
cylindrica as template to form interconnected macrostructure pores. Fig 1 shows the
green bodies before sintering and after sintering processes.

Fig.1 Before Sintering (a); After Sintering (b)

Figure 1 shows that volume samples has been decreased. The volume was
decreasing because of densification when sintering processes [Kang, 2005], the
densification caused the matrix of bodies dense along with the loss of organic
compound [Li et al, 2013].

3.2 Shrinkage of bodies HA scaffold


3.2.1 Influence of darvan 821A addition
Fig 2 shows the effect of darvan 821A on shrinkage of HA scaffold. When
the darvan 821A increased from 2% to 3%wt, the shrinkage decreased from
40.84 to 27.75 vol.%. The increasing of darvan 812A causing increased of
matrix organic in the slurry, when these matrix organic burned at 600 oC that
makes the samples lost itself volume along densifications during sintering
process [Kang, 2005].
Fig.2 Effect of darvan 821A on shrinkage of HA scaffolds

3.2.2 Influence of solid loading addition


Fig. 3 shows the effect of solid loading on shrinkage of HA scaffolds. The
increasing of HA loading decreased shrinkage. When HA loading was
increasing from 10 to 12 g, the shrinkage decreased from 57.91 to 53.62 vol.%.
The increased of ceramic solid loading causing more amount of solids in the
slurry, the higher solids concentration in the slurry will reduce shrinkage and
prevent the occurrence of cracks on the surface of the ceramic body [Fadli and
Komalasari, 2013].
Fig.3 Effect of solid loading on shrinkage of HA scaffolds

The shrinkage is the decreased of sintered bodies volume which lost along
the densification process. The shrinkage of sintered bodies lead to increased
pore density and mechanical properties materials. The increased of sintering
temperature also causing greater shrinkage. Rising temperatures increased the
rate of densification of samples so that causing the particles become denser
[Kang, 2005]. Sintering below HA scaffold melting point make the particles
densified well and resulted in smaller pore sizes and denser walls. Thus, the
shrinkage increased [Fadli et al, 2015].

3.3 Porosity of HA Scaffold


3.3.1 Influence of Darvan 821A Addition
Basically, the addition of darvan 821A is for maintaining the quality of
slurry and avoiding the deposition of solid loading [Zhang, 2003]. The density
of HA scaffold increased along darvan 821A addition. The increasing of
density caused by darvan 821A addition that makes the slurries more viscous
and it was finally maintained the colloidal properties of the slurries which
makes the sintered bodies has greater structure.
Fig.4 Effect of Darvan 821A Addition on Porosity of HA Scaffold

The addition of darvan 821A, decreasing the porosity of materials. When


darvan 821A increased from 2% to 3%wt, the porosity decreased from 64.80%
to 58.74%. Figure 4 shows that the porosity decreasing along the addition of
darvan 821A. Fu et al [2007] mentioned the addition of dispersing agent
reducing the formation of flocculation in suspension, it causing the suspension
has a great colloidal properties stability which makes the suspension can stand
the template and resulted lower porosity after sintering process.

3.3.1 Influence of solid loading addition


Figure shows effect of HA loading addition towards porosity scaffold.
When the addition of solid loading increasing from 10 to 12 g, the porosity
decreased from 56.51 to 53.26%. The decreasing of porosity caused by
densification during sintering process. The decreased porosity declare that
material structure more compact because densification process and makes the
density increased. The increasing of density causing reduction of porous and
finally decreased of material porosity [Kang, 2005].
Fig.5 Effect of Darvan 821A Addition on Porosity of HA Scaffold

3.4 Compressive Strength and Morphology of HA scaffold


Figure 7 (a) shows effect darvan 821A addition towards compressive strength of
HA scaffold. When the darvan 821A increased from 2% to 3%wt, the compressive
strength increased from 2.03 to 2.42 MPa. the increased of compressive strength
investigated affected by reduction of porosity. Rahman and Guan [2007] mentioned
that the lower compressive strength affected by size and degree of porosity.

a b

Fig. 7 Effect of Darvan 821A on Compressive Strength of HA scaffold with 10 g


HA Loading Addition (a); Microstructure of HA Scaffold with 0.2 g Darvan 821A
Addition (b);

Figure 7 (b) shows the microstructure of HA Scaffold has been made at an addition
of 0.3 g darvan 821A. The addition of 0.3 g darvan 821A causing astablishment of
dense porous stucture and well-interconected porous between each porous. The
addition of darvan 821A can defend itself koloidal characteristic and its make the
slurries cling over the templates and forming the indentical shape with the template.
Figure 8 (a) shows effect of HA loading addition on compressive strength of HA
scaffold. Figure below shows compressive strength increasing along the increasing
of HA loading addition. When the HA loading increased from 10 to 12 g, the
compressive strength increased from 3.59 to 7.09 MPa. based on swain et al [2011]
the increased of compressive strength caused by the addition of HA loading, the
addition of HA loading produced viscous slurries which has higher particles
interaction and resulted the compressive strength increased.

Fig. 8 Effect of HA Loading on Compressive Strength of HA scaffold with 0.3 g


Darvan 821A Addition (a); Microstructure of HA Scaffold with 10 g Solid Loading
Addition (b)

Figure 8 (b) shows microstructure of HA scaffold which form by an addition of 10


g HA loading and 0.3 g darvan 821A. that shows the addition of HA loading
causing well-interconected and denser pores structure. The compressive strength is
strongly affected by the struts and the surface defect of the strut. The strength of
strut depend on solid loading ceramic [ Jamaludin et al, 2015]

Fig.9 Addition 0.3 g of Darvan 821A (a); Addition 12 g of Solid Loading (b)
Figure 9 shows the result of scanning electron macroscopic of HA scaffolds. The
scaffold has pore size in the range of 50-400 m. Based on figure 9 (a) and 9 (b), it
can be seen that the addition of darvan 821A and HA loading have differences pores
structures. Figure 9 (a) and 9 (b) have compressive strength each are 2.42 and 7.09
MPa. The results are in accordance with studies by Rahman and Guan [2007] which
declare that the decreased of degree and pores size leads to greater compressive
strength.

4. Conclusion
HA scaffold has been made by utilizing Luffa cylindrica as a template. The increased
of Darvan 821A and HA loading in the slurry leads to lower shrinkage and porosity,
and higher density and compressive strength. HA scaffold has lowest shrinkage by
addition of Darvan 821A is 27.75 vol.%; lowest porosity by addition of HA loading
is 53.26%; higest density by addition of HA loading is 1.48%; and highest
compressive strength by addition of HA loading is 7.09 MPa.

Acknowledgement
This work was supported by University of Riau.

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