International Journal of Engineering and Science Vol. 1, No. 1, 2010 ISSN: 2086-3799 Available online at: www.univ-malahayati.ac.

id/ijes 2010 Universitas Malahayati Press

Egg Yolk as Pore Creating Agent for Porous Tri-Calcium Phosphate

A.R. Fariza, A. Zuraida, I.Sopyan
Department of Manufacturing and Materials Engineering, Faculty of Engineering, International Islamic University Malaysia (IIUM), Jalan Gombak, 53100 Kuala Lumpur, Malaysia.

Abstract
Porous tri-calcium phosphate which is to be applied as artificial bone was prepared via protein consolidation method and egg yolk is used to give binding effect as well as to create porosity. In this experiment, fractions of egg yolk is controlled from 50 wt%, 60 wt%, 70wt% and 80 wt% and the mixture of egg yolk and tri-calcium phosphate powder were dried at 60 C before undergone uniaxial compaction method. Subsequently, pressure of 68.5 MPa is given to the mold to produce cylindrical shape samples with diameter to height ratio of 1:2. Samples were then sintered at 1100C to achieve porous tri-calcium phosphate. This method produces porous tri-calcium phosphate with desired porosity of 20-54.5% and acceptable compressive strength between 0.7-0.07 MPa. Besides, microporosity of 0.4-1m and macroporosity in the range of 100-800m were successfully obtained from this method.
KEYWORDS: Porous tri-calcium phosphate, egg yolk, porosity, compressive strength

1.

Introduction

There are a lot of concerns have been put in order for the researchers to consider the best way to respond to the demand on the biomaterials products since there are a lot of shortcomings derived from allograft and autograft as bone substitutes. They tried to discover as simple as possible method plus reducing in cost as an advantage. Besides, the usage of environmental-friendly materials should also be considered as it becomes the main concern nowadays. Then again, the produced artificial bones must meet several criteria before it can be applied to human body. These are the major challenges for the researchers in order to develop porous artificial bone with desired porosity and acceptable mechanical strength. For synthetic bone applications, bioceramics from calcium phosphate family is often used due to its properties that mimic the natural human bone. However, hydroxyapatite (HA) and tricalcium phosphate (TCP) are the most favorable because of their good biocompatibility and osteointegrative properties [1]. When comparison is made between these two bioceramics, TCP has more preferences for the reason that it dissolves and resorbs much more quickly than HA. Moreover, HA shows almost no absorption and remains in the body for a long time as foreign substances [2]. In order for the artificial bone to be accommodated by the host tissues, it must exhibit porosity as to encourage cell growth within the three dimensional structure. Yet, the pores must be interconnected to each other in order to mimic the architecture of the mineral phase of living bone [3]. Previously, there are many
Corresponding Author:

inspired ways of producing porous artificial bones such as by polymeric sponge method and conversion of marine coral skeleton. Alternatively, as the porosity of the artificial bone needs to be controlled, researchers nowadays are using pore creating agents either organic or inorganic materials to achieve the desired porosity. Examples of the prominent pore creating agents are polymethylmethacrylate micro beads (PMMA), sodium chloride (NaCl), carbon beads, starch, ice and naphthalene. In general, these pore creating agents will decomposed from the prepared samples during sintering thus creating the porosities [4-6]. The employment of egg yolk as emulsifier in food industry promotes the idea that it can be an excellent binder plus creating porosity when heated. Normally in food production, proteins in yolk coagulate and form a solid or semisolid structure when exposed to heat at the temperature between 60- 70C. This feature turns egg yolk to be a desired binder that holds elements together. Besides, its readily available film-forming properties preserve the moisture between particles [7]. From these unique properties of egg yolk, micro and macro- porosity is expected to be present in sintered TCP together with interconnecting porosity as to mimic human natural bones. This paper demonstrates the possibility of applying controlled fractions of egg yolk as binder and pore creating agent to develop porous TCP via protein consolidation method with desired porosity and satisfactory compressive strength.

Fariza bt Abdul Rahman, Department of Manufacturing and Materials Engineering, Faculty of Engineering. International Islamic University Malaysia, Jalan Gombak, 53100, Kuala Lumpur, Malaysia, Tel: +603-6196-4487, Fax: +603-6196-4433, E-mail: mizz_eman@yahoo.com

A.R. Fariza, et al / Int. J. Eng and Sci.. Vol. 1, No. 1, 2010, 9 - 12 2. Experimental

In this experiment, commercial powder of TCP (R & M Marketing, UK) is mixed manually with controlled fraction of commercial egg yolk (50wt%, 60wt%, 70wt% and 80wt %) homogenously. In order to undergone uniaxial hydraulic press, the mixture needs to be in dry form. Thus, it was dried in the oven at 60C for 24 hours. After drying, the mixture is crushed manually by using mortar and pastel. For shaping process, uniaxial hydraulic press was used with the pressure of 68.5MPa. This process produced cylindrical shape samples with diameter to height ratio of 1:2. The prepared samples were subsequently heated at 600C with the rate of 5C/min and 3 hours holding time to remove the egg yolk. This process was then continued with heating at 1100C at the rate of 10C/min followed by 3 hours holding time. In order to determine the volume shrinkage, volume of the samples was measured before and after sintering process was done. Then again, the porosity was calculated from the apparent and relative densities of the sintered samples. The compressive strength of these samples was evaluated by using INSTRON Universal (8874) testing machine at the speed of 1mm min-1. Finally samples macroporosity was observed via JEOL JSM 5600 Scanning Electron Microscope (SEM) while JEOL JSM 6700F Field Emission Scanning Electron Microscope (FESEM) is used to examine the microporosity. Table 1. Samples preparation. Sample Fraction of egg yolk (wt %) A 50 B 60 C 70 D 80 3. Results and discussion

Figure1. TGA diagram of commercial egg yolk. Volume shrinkage of the fabricated samples increases exponentially ranging from 6.2- 38.6 vol. % as in Figure 2. On the other hand, due to the large amount of egg yolk decomposed during heating, sample D shows almost 26% additional shrinkage compared to sample A, B and C. In addition, sample D tends to change its shape and shows some distortions after sintering.

Fraction of TCP powder (wt %) 50 40 30 20

Figure2. Sintering shrinkage of porous TCP. The inverse relationship between ceramics porosity and its compressive strength is proven in Table 2 as it verified that an increment in porosity causes declination in the compressive strength. As more amount of egg yolk is added, the porosity increases from 20 to 54.5% but the compressive strength decreases from 0.7 to 0.07 MPa which is 90% in value difference. The compressive strength attained from this method shows comparable results with freeze drying technology which create porosity by the sublimation of ice [9]. Table 2. Characteristics of sintered TCP samples. Sample Porosity Compressive (%) Strength (MPa) A 20.3 0.70 B 24.5 0.12 C 34.8 0.09 D 54.5 0.07

Figure 1 shows TGA diagram for commercial egg yolk. There are two stages can be observed from this figure. At the temperature of 150C, the graph demonstrates weight loss of 50% with slow decomposition process. This is the temperature where water inside egg yolk evaporates and thus reducing its weight. The second stage occurs at temperature of 450C with 94% weight loss is observed. From this TGA data obtained, the temperature of 600C with 3 hours holding time plus slow heating rate of 5C/min is the most suitable to be used in the sintering process to completely remove the egg yolk from the compacted body [8].

12

Figure 3. FESEM morphology of microcoposity for; (a) sample A (b) sample B (c) sample C (d) sample D In Figure 3, FESEM morphology of the samples demonstrates the morphology of microporosity ranging from 0.4 to 1 m for all samples. This microporosity is highly desired to help the diffusion process of calcium and phosphorus ions for mineralization [10]. Micropososity can be greatly obtained as increase in egg yolk fractions. Moreover, the size of the porosity is also growing from sample A to D. However, macroporosity can only be observed from sample C and D since the fraction of egg yolk is enough to create desired macroporosity. For bone application, macroporosity in the range of 100800m as in Figure 4 is needed to host the cellular and extracellular components of bones also to be effective for osteoconduction [5]. Furthermore, both figures proved the existence of interconnectivity between pores which will allow the penetration of the osteoblast-like cells inside the pores [11].

Figure 4: SEM pictures of macroporosity for sample C (left) and D (right).

4.

Conclusion

This simple protein consolidation method by using egg yolk as organic binder and pore creating agent has successfully produced porous TCP with 2054.5% porosity as well as compressive strength of 0.7-0.07 MPa. Moreover, egg yolk as pore creating agents has effectively produced microporosity from 0.4- 1m together with macroporosity of 100-800m. References [1] S. Amit, A. Ingle, K.R. Munim S.N. Vaidya, B.P. Sharma, A.N. Bhisey. (2001). Development of calcium phosphate based bioceramics, Bulletin Materials Science, 24 653-657. J.F. Keating, M.M. McQueen. (2001). Substitute for autologous bone graft in orthopedic trauma. The Journal of Bone and Joint Surgery, 82 3-8. B. Flautre, M. Descamps, C. Delecourt, M.C. Blary, P. Hardouin. (2001) Porous HA Ceramic for bone replacement: Role of the pores and interconnections- Experimental study in the rabbit. Journal of Materials Science: Materials in Medicine, 12 679-68. I.Sopyan, M. Mel, S. Ramesh, K.A. Khalid. (2007). Porous hydroxyapatite for artificial

[2]

[3]

[4]

bone applications. Science and Technology of Advanced Materials, 8 116-123. [5] X. Yao, S. Tan, D. Jiang. (2005). Improving the properties of porous hydroxyapatite ceramics by fabricating methods. Journal of Materials Science, [6] K. Pal, S. Pal. (2006). Development of porous hydroxyapatite scaffolds. Materials and Manufacturing Processes, 21 325-328 [7] A.K. Lynn. (1999). The egg and the equivalent-part two, Weeks Publishing Company, [8] K. Prabhakaran, Anand Melkeri, N.M. Gokhale, S.C. Sharma. (2007). Preparation of macroporous alumina ceramics using wheat particles as gelling and pore forming agent, Ceramics International, 33 77-81. [9] L. Luilan, J. Shaohua, Z. Huicun, H. Qingxi, Fabrication of porous -tcp scaffolds by comnation of rapid prototyping and freeze drying technology, IFMBE Proceedings, 19 [10] K. Nursen, T. Muharrem, K. Feza. (2004). Fabrication and characterization of porous tricalcium phosphate ceramics, Ceramics International, 30 205-211. [11] I. Sopyan, J. Kaur, A.R. Toibah, M. Hamdi, S. Ramesh. (2008). Effect of slurry preparation on physical properties of porous hydroxyapatite prepared via polymeric sponge method, Advanced Materials Research, 47-50 932-935.