HAKAN OFLAZ, Betül ALDEMİR DİKİCİ, Serkan DİKİCİ1

The Effect of Heat Treatment on Physical, Chemical and Structural Properties of Calcium Sulfate Based Scaffolds

3D printed calcium sulfate (CS) is a promising material for on custom bone substitutes. Since it dissolves easily in body fluids, manufactured samples require to being improved to reduce solubility. The main aim of this study was reducing the dissolubility of CS based samples by using sintering and investigating the effect of heat treatment on their physical, chemical and structural properties. To observe the effect of heat treatment on samples, contact angles were measured, X-Ray diffraction analysis (XRD) was performed, and scanning electron microscope (SEM) micrographs were captured before and after the sintering process, and the results were compared. Furthermore, sintered and non-sintered samples were soaked in phosphate buffered saline (PBS) to observe the impact of sintering on the solubility of the material. Also, three different pore sized scaffolds were manufactured to test the limits of the 3D printer for manufacturing of scaffolds with open pores. Sintering process results in a volume reduction and according to SEM results, CS grains were fused together after heat treatment. Although non-sintered CS sample starts to dissolve in high rate and nearly 1/3 of the sample was at the bottom of the glass in a matter of minutes, sintering creates more rigid structure and there were not visible dissolution in PBS at the end of a week. The contact angle of samples cannot be measured, so it can be concluded that 3D printed material showed a super-hydrophilic property. XRD diagram suggested that there is not any new phase created in the printing and sintering processes except related hydrates of CS. As a result of the 3D printing, 500 µm, 750 µm and 1000 µm pore sized scaffolds were manufactured, successfully. However, it was seen that 500 µm pores could not be open by using depowdering after the printing process.

Anahtar Kelimeler:

Tissue engineering, Calcium sulfate; Sintering; 3 Dimensional printing; Biomedical

PDF

___

[1] Bose, S., Roy, M., Bandyopadhyay, A. Recent advances in bone tissue engineering scaffolds. Trends in biotechnology, 30(2012), 546-54.
[2] Rauh, J., Milan, F., Gunther, K.P., Stiehler, M. Bioreactor systems for bone tissue engineering. Tissue engineering. Part B, Reviews, 17(2011), 263-80.
[3] Brydone, A.S., Meek, D., Maclaine, S. Bone grafting, orthopaedic biomaterials, and the clinical need for bone engineering. Proceedings of the Institution of Mechanical Engineers. Part H, Journal of engineering in medicine, 224(2010), 1329-43.
[4] Lichte, P., Pape, H.C., Pufe, T., Kobbe, P., Fischer, H. Scaffolds for bone healing: concepts, materials and evidence. Injury, 42(2011), 569-73.
[5] Inzana, J.A., Olvera, D., Fuller, S.M., Kelly, J.P., Graeve, O.A., Schwarz, E.M., et al. 3D printing of composite calcium phosphate and collagen scaffolds for bone regeneration. Biomaterials, 35(2014), 4026-34.
[6] Subia, B.K., J.; Kundu, S. C. . Biomaterial Scaffold Fabrication Techniques for Potential Tissue Engineering Applications. In: Tissue Eng, Eberli, D. Ed., 2010.
[7] Wu, H.D., Lee, S.Y., Poma, M., Wu, J.Y., Wang, D.C., Yang, J.C. A Novel Resorbable α-Calcium Sulfate Hemihydrate/Amorphous Calcium Phosphate Bone Substitute for Dental Implantation Surgery. Materials Science and Engineering C, 32(2012).
[8] Thomas, M.V., Puleo, D.A., Al-Sabbagh, M. Calcium sulfate: a review. Journal of long-term effects of medical implants, 15(2005), 599-607.
[9] Pietrzak, W.S., Ronk, R. Calcium sulfate bone void filler: a review and a look ahead. The Journal of craniofacial surgery, 11(2000), 327-33; discussion 34.
[10] Sidqui, M., Collin, P., Vitte, C., Forest, N. Osteoblast adherence and resorption activity of isolated osteoclasts on calcium sulphate hemihydrate. Biomaterials, 16(1995), 1327-32.
[11] al Ruhaimi, K.A. Effect of calcium sulphate on the rate of osteogenesis in distracted bone. International journal of oral and maxillofacial surgery, 30(2001), 228-33.
[12] Utela, B., Storti, D., Anderson, R., Ganter, M. A Review of Process Development Steps for New Material Systems in Three Dimentional Printing (3DP). Journal of Manufacturing Processes, 10(2008).
[13] Chen, Z.G., Liu, H.Y., Liu, X., Lian, X.J., Guo, Z.W., Jiang, H.J., et al. Improved workability of injectable calcium sulfate bone cement by regulation of self-setting properties. Mat Sci Eng C-Mater, 33(2013), 1048-53.
[14] Bose, S., Vahabzadeh, S., Bandyopadhyay, A. Bone tissue engineering using 3D printing. Mater Today, 16(2013), 496-504.
[15] Suwanprateeb, J., Sanngam, R., Suvannapruk, W., Panyathanmaporn, T. Mechanical and in vitro performance of apatite-wollastonite glass ceramic reinforced hydroxyapatite composite fabricated by 3D-printing. Journal of materials science. Materials in medicine, 20(2009), 1281-9.
[16] Khalyfa, A., Vogt, S., Weisser, J., Grimm, G., Rechtenbach, A., Meyer, W., et al. Development of a new calcium phosphate powder-binder system for the 3D printing of patient specific implants. Journal of materials science. Materials in medicine, 18(2007), 909-16.
[17] Asadi-Eydivand, M., Solati-Hashjin, M., Shafiei, S.S., Mohammadi, S., Hafezi, M., Abu Osman, N.A. Structure, Properties, and In Vitro Behavior of Heat-Treated Calcium Sulfate Scaffolds Fabricated by 3D Printing. PloS one, 11(2016), e0151216.
[18] Aldemir, B. Development, Production and Characterization of Ceramic Based 3D Tissue Scaffolds. Izmır, Izmir Katip Celebi University; 2016.
[19] Asadi-Eydivand, M., Solati-Hashjin, M., Farzad, A., Abu Osman, N.A. Effect of technical parameters on porous structure and strength of 3D printed calcium sulfate prototypes. Robot Cim-Int Manuf, 37(2016), 57-67.
[20] Teoreanu, I., Preda, M., Melinescu, A. Synthesis and characterization of hydroxyapatite by microwave heating using CaSO4.2H2O and Ca(OH)2 as calcium source. Journal of materials science. Materials in medicine, 19(2008), 517-23.
[21] Iribarne, A.P.I.J.V.A.A.J. Reactivity of calcium sulfatefrom FBC systems Fuel, 76(1997).
[22] Marsh, D.V.U., D. L. Rate And Diffusional Study Of The Reaction Of Calcium Oxide With Sulfur Dioxide. Chemical EngineeringScience, 40(1985).
[23] Zhou, Z., Buchanan, F., Mitchell, C., Dunne, N. Printability of calcium phosphate: calcium sulfate powders for the application of tissue engineered bone scaffolds using the 3D printing technique. Materials science & engineering. C, Materials for biological applications, 38(2014), 1-10.
[24] Anselme, K. Osteoblast adhesion on biomaterials. Biomaterials, 21(2000), 667-81.
[25] Yamada, N., Okano, T., Sakai, H., Karikusa, F., Sawasaki, Y., Sakurai, Y. Thermoresponsive Polymeric Surfaces - Control of Attachment and Detachment of Cultured-Cells. Makromol Chem-Rapid, 11(1990), 571-6.